# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_me160616w1_vinklarek
_database_code_depnum_ccdc_archive 'CCDC 1914035'
loop_
_audit_author_name
_audit_author_address
'Ivana Cisarova'
;Charles Univerzity
Czech Republic
;
_audit_update_record             
;
2019-05-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H26 N4 O4 P2 Si W'
_chemical_formula_sum            'C18 H26 N4 O4 P2 Si W'
_chemical_formula_weight         636.31
_chemical_compound_source        'synthesized by the authors'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.9717(10)
_cell_length_b                   20.3377(9)
_cell_length_c                   21.9312(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.5880(10)
_cell_angle_gamma                90
_cell_volume                     10226.0(8)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9949
_cell_measurement_theta_min      2.2464
_cell_measurement_theta_max      27.5286

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             4992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.226
_exptl_absorpt_coefficient_mu    4.719
_shelx_estimated_absorpt_T_min   0.232
_shelx_estimated_absorpt_T_max   0.415
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS  micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            131565
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.112
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             23576
_reflns_number_gt                19672
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.1'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+11.9338P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.000215(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         23576
_refine_ls_number_parameters     1127
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0505
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.65582(2) 0.23926(2) 0.32059(2) 0.01751(3) Uani 1 1 d . . . . .
P11 P 0.69343(3) 0.31150(3) 0.24500(3) 0.01820(13) Uani 1 1 d . . . . .
P12 P 0.62280(3) 0.16674(3) 0.23866(3) 0.01748(12) Uani 1 1 d . . . . .
Si1 Si 0.66549(3) 0.23594(3) 0.11858(3) 0.01505(13) Uani 1 1 d . . . . .
N11 N 0.71609(9) 0.34891(10) 0.13722(9) 0.0212(4) Uani 1 1 d . . . . .
N12 N 0.68943(9) 0.29951(10) 0.16934(9) 0.0182(4) Uani 1 1 d . . . . .
N13 N 0.60486(9) 0.12898(10) 0.12773(9) 0.0209(4) Uani 1 1 d . . . . .
N14 N 0.62974(9) 0.17825(10) 0.16424(9) 0.0177(4) Uani 1 1 d . . . . .
C12 C 0.72980(11) 0.38267(12) 0.23793(12) 0.0219(5) Uani 1 1 d . . . . .
H12 H 0.742746 0.410676 0.270691 0.026 Uiso 1 1 calc R U . . .
C13 C 0.73802(11) 0.39414(12) 0.17538(11) 0.0200(5) Uani 1 1 d . . . . .
C14 C 0.58105(10) 0.08413(12) 0.16198(11) 0.0186(5) Uani 1 1 d . . . . .
C15 C 0.58654(11) 0.09536(12) 0.22550(11) 0.0202(5) Uani 1 1 d . . . . .
H15 H 0.572223 0.067421 0.255886 0.024 Uiso 1 1 calc R U . . .
C16 C 0.76854(12) 0.45384(13) 0.15049(12) 0.0274(6) Uani 1 1 d . . . . .
C17 C 0.82486(15) 0.46643(19) 0.18843(19) 0.0570(11) Uani 1 1 d . . . . .
H17A H 0.850948 0.428622 0.185272 0.086 Uiso 1 1 calc R U . . .
H17B H 0.816309 0.472907 0.231239 0.086 Uiso 1 1 calc R U . . .
H17C H 0.843738 0.505905 0.173321 0.086 Uiso 1 1 calc R U . . .
C18 C 0.72986(16) 0.51371(17) 0.1578(2) 0.0730(15) Uani 1 1 d . . . . .
H18A H 0.750828 0.553419 0.146519 0.110 Uiso 1 1 calc R U . . .
H18B H 0.719620 0.517106 0.200388 0.110 Uiso 1 1 calc R U . . .
H18C H 0.694207 0.509146 0.131162 0.110 Uiso 1 1 calc R U . . .
C19 C 0.7814(2) 0.4435(2) 0.08500(18) 0.0834(14) Uani 1 1 d . U . . .
H19A H 0.802402 0.481814 0.070367 0.125 Uiso 1 1 calc R U . . .
H19B H 0.744781 0.437937 0.060210 0.125 Uiso 1 1 calc R U . . .
H19C H 0.805561 0.404115 0.081625 0.125 Uiso 1 1 calc R U . . .
C110 C 0.55008(11) 0.02644(12) 0.12955(12) 0.0229(5) Uani 1 1 d . . . . .
C111 C 0.59387(13) -0.00977(15) 0.09174(15) 0.0379(7) Uani 1 1 d . . . . .
H11A H 0.626124 -0.026281 0.118864 0.057 Uiso 1 1 calc R U . . .
H11B H 0.609100 0.020548 0.061873 0.057 Uiso 1 1 calc R U . . .
H11C H 0.574401 -0.046747 0.070298 0.057 Uiso 1 1 calc R U . . .
C112 C 0.50028(13) 0.05243(15) 0.08637(14) 0.0339(7) Uani 1 1 d . . . . .
H11D H 0.481563 0.015610 0.063977 0.051 Uiso 1 1 calc R U . . .
H11E H 0.515926 0.083429 0.057347 0.051 Uiso 1 1 calc R U . . .
H11F H 0.471524 0.074859 0.110177 0.051 Uiso 1 1 calc R U . . .
C113 C 0.52557(15) -0.02065(14) 0.17549(14) 0.0379(7) Uani 1 1 d . . . . .
H11G H 0.557541 -0.038294 0.202322 0.057 Uiso 1 1 calc R U . . .
H11H H 0.505306 -0.056857 0.153658 0.057 Uiso 1 1 calc R U . . .
H11I H 0.498099 0.002920 0.200038 0.057 Uiso 1 1 calc R U . . .
C114 C 0.72980(11) 0.19674(14) 0.08879(13) 0.0276(6) Uani 1 1 d . . . . .
H11J H 0.751783 0.229360 0.066690 0.041 Uiso 1 1 calc R U . . .
H11K H 0.717333 0.161025 0.060956 0.041 Uiso 1 1 calc R U . . .
H11L H 0.754650 0.178911 0.122797 0.041 Uiso 1 1 calc R U . . .
C115 C 0.61300(13) 0.26827(14) 0.06003(13) 0.0315(6) Uani 1 1 d . . . . .
H11M H 0.578476 0.284538 0.079377 0.047 Uiso 1 1 calc R U . . .
H11N H 0.601483 0.233241 0.031051 0.047 Uiso 1 1 calc R U . . .
H11O H 0.630888 0.304378 0.038268 0.047 Uiso 1 1 calc R U . . .
C116 C 0.73408(12) 0.19151(13) 0.32488(12) 0.0248(6) Uani 1 1 d . . . . .
C117 C 0.62357(13) 0.17719(13) 0.38136(12) 0.0277(6) Uani 1 1 d . . . . .
C118 C 0.68339(13) 0.29789(13) 0.39038(12) 0.0281(6) Uani 1 1 d . . . . .
C119 C 0.57838(12) 0.28916(13) 0.31111(11) 0.0244(5) Uani 1 1 d . . . . .
O11 O 0.77810(9) 0.16530(11) 0.32567(10) 0.0408(5) Uani 1 1 d . . . . .
O12 O 0.60537(11) 0.14218(11) 0.41617(10) 0.0447(6) Uani 1 1 d . . . . .
O13 O 0.69877(11) 0.32985(10) 0.43089(9) 0.0447(6) Uani 1 1 d . . . . .
O14 O 0.53546(9) 0.31717(11) 0.30470(9) 0.0378(5) Uani 1 1 d . . . . .
W2 W 0.41672(2) 0.25671(2) 0.43083(2) 0.01806(3) Uani 1 1 d . . . . .
P21 P 0.45635(3) 0.18757(3) 0.51208(3) 0.01863(13) Uani 1 1 d . . . . .
P22 P 0.37691(3) 0.32592(3) 0.50729(3) 0.01833(13) Uani 1 1 d . . . . .
Si2 Si 0.41465(3) 0.25465(3) 0.63373(3) 0.01621(13) Uani 1 1 d . . . . .
N21 N 0.47500(9) 0.14814(10) 0.62246(9) 0.0208(4) Uani 1 1 d . . . . .
N22 N 0.44787(9) 0.19653(10) 0.58663(9) 0.0186(4) Uani 1 1 d . . . . .
N23 N 0.35757(9) 0.36360(10) 0.61576(9) 0.0210(4) Uani 1 1 d . . . . .
N24 N 0.38408(9) 0.31507(10) 0.58289(9) 0.0176(4) Uani 1 1 d . . . . .
C22 C 0.49637(11) 0.11904(12) 0.52431(11) 0.0216(5) Uani 1 1 d . . . . .
H22 H 0.512894 0.093376 0.493590 0.026 Uiso 1 1 calc R U . . .
C23 C 0.50141(10) 0.10584(12) 0.58750(11) 0.0190(5) Uani 1 1 d . . . . .
C24 C 0.33290(10) 0.40770(12) 0.57783(11) 0.0186(5) Uani 1 1 d . . . . .
C25 C 0.33864(11) 0.39570(12) 0.51523(11) 0.0206(5) Uani 1 1 d . . . . .
H25 H 0.323367 0.422669 0.482675 0.025 Uiso 1 1 calc R U . . .
C26 C 0.53190(11) 0.04723(13) 0.61823(12) 0.0234(5) Uani 1 1 d . . . . .
C27 C 0.57323(13) 0.01462(14) 0.57515(14) 0.0328(7) Uani 1 1 d . . . . .
H27A H 0.550948 -0.000401 0.538190 0.049 Uiso 1 1 calc R U . . .
H27B H 0.592429 -0.023064 0.595705 0.049 Uiso 1 1 calc R U . . .
H27C H 0.602756 0.046476 0.563984 0.049 Uiso 1 1 calc R U . . .
C28 C 0.48484(14) -0.00190(14) 0.63438(16) 0.0385(7) Uani 1 1 d . . . . .
H28A H 0.459445 0.018371 0.663355 0.058 Uiso 1 1 calc R U . . .
H28B H 0.503328 -0.041114 0.652918 0.058 Uiso 1 1 calc R U . . .
H28C H 0.461584 -0.014413 0.597197 0.058 Uiso 1 1 calc R U . . .
C29 C 0.56689(14) 0.06909(15) 0.67654(14) 0.0376(7) Uani 1 1 d . . . . .
H29A H 0.597768 0.099473 0.665872 0.056 Uiso 1 1 calc R U . . .
H29B H 0.584386 0.030531 0.697268 0.056 Uiso 1 1 calc R U . . .
H29C H 0.540884 0.091242 0.703739 0.056 Uiso 1 1 calc R U . . .
C210 C 0.30304(11) 0.46645(13) 0.60524(12) 0.0235(5) Uani 1 1 d . . . . .
C211 C 0.26918(14) 0.50596(15) 0.55534(14) 0.0380(7) Uani 1 1 d . . . . .
H21A H 0.296270 0.522727 0.526249 0.057 Uiso 1 1 calc R U . . .
H21B H 0.249420 0.542920 0.573925 0.057 Uiso 1 1 calc R U . . .
H21C H 0.240168 0.477529 0.533899 0.057 Uiso 1 1 calc R U . . .
C212 C 0.34914(13) 0.51065(15) 0.63720(16) 0.0395(8) Uani 1 1 d . . . . .
H21D H 0.370470 0.485897 0.669789 0.059 Uiso 1 1 calc R U . . .
H21E H 0.330150 0.548735 0.654801 0.059 Uiso 1 1 calc R U . . .
H21F H 0.376413 0.525701 0.607540 0.059 Uiso 1 1 calc R U . . .
C213 C 0.26003(14) 0.44181(15) 0.65102(14) 0.0368(7) Uani 1 1 d . . . . .
H21G H 0.231220 0.412759 0.630058 0.055 Uiso 1 1 calc R U . . .
H21H H 0.240077 0.479431 0.668272 0.055 Uiso 1 1 calc R U . . .
H21I H 0.281356 0.417532 0.683922 0.055 Uiso 1 1 calc R U . . .
C214 C 0.35530(13) 0.21492(14) 0.67171(14) 0.0338(7) Uani 1 1 d . . . . .
H21J H 0.326555 0.197658 0.640889 0.051 Uiso 1 1 calc R U . . .
H21K H 0.336537 0.247096 0.697346 0.051 Uiso 1 1 calc R U . . .
H21L H 0.371023 0.178730 0.697243 0.051 Uiso 1 1 calc R U . . .
C215 C 0.47139(13) 0.29182(14) 0.68457(13) 0.0320(6) Uani 1 1 d . . . . .
H21M H 0.485746 0.259374 0.714940 0.048 Uiso 1 1 calc R U . . .
H21N H 0.455235 0.329678 0.705398 0.048 Uiso 1 1 calc R U . . .
H21O H 0.503657 0.306371 0.660664 0.048 Uiso 1 1 calc R U . . .
C216 C 0.49084(12) 0.31295(14) 0.43734(12) 0.0258(6) Uani 1 1 d . . . . .
C217 C 0.38183(12) 0.31309(13) 0.36247(12) 0.0265(6) Uani 1 1 d . . . . .
C218 C 0.45184(13) 0.19849(14) 0.36880(12) 0.0302(6) Uani 1 1 d . . . . .
C219 C 0.34291(13) 0.20029(14) 0.42941(12) 0.0289(6) Uani 1 1 d . . . . .
O21 O 0.53181(9) 0.34443(11) 0.44209(10) 0.0409(5) Uani 1 1 d . . . . .
O22 O 0.36174(10) 0.34395(11) 0.32318(9) 0.0423(5) Uani 1 1 d . . . . .
O23 O 0.47203(12) 0.16556(11) 0.33370(10) 0.0513(7) Uani 1 1 d . . . . .
O24 O 0.30219(10) 0.16829(12) 0.43028(10) 0.0448(6) Uani 1 1 d . . . . .
W3 W 0.18674(2) 0.24324(2) 0.29743(2) 0.01887(3) Uani 1 1 d . . . . .
P31 P 0.21036(3) 0.32112(3) 0.21943(3) 0.01951(13) Uani 1 1 d . . . . .
P32 P 0.14365(3) 0.17496(3) 0.21653(3) 0.02008(13) Uani 1 1 d . . . . .
Si3 Si 0.16162(3) 0.25589(3) 0.09358(3) 0.02105(15) Uani 1 1 d . . . . .
N31 N 0.21668(10) 0.36605(11) 0.11082(10) 0.0261(5) Uani 1 1 d . . . . .
N32 N 0.19467(9) 0.31483(10) 0.14415(9) 0.0217(4) Uani 1 1 d . . . . .
N33 N 0.11219(9) 0.14287(11) 0.10635(10) 0.0242(5) Uani 1 1 d . . . . .
N34 N 0.13929(9) 0.19195(11) 0.14176(9) 0.0224(5) Uani 1 1 d . . . . .
C32 C 0.24649(11) 0.39237(12) 0.21065(12) 0.0227(5) Uani 1 1 d . . . . .
H32 H 0.264754 0.417808 0.242757 0.027 Uiso 1 1 calc R U . . .
C33 C 0.24522(11) 0.40808(13) 0.14790(12) 0.0234(5) Uani 1 1 d . . . . .
C34 C 0.09614(11) 0.09427(12) 0.14137(12) 0.0221(5) Uani 1 1 d . . . . .
C35 C 0.10965(11) 0.10210(13) 0.20473(12) 0.0238(5) Uani 1 1 d . . . . .
H35 H 0.101022 0.071424 0.235557 0.029 Uiso 1 1 calc R U . . .
C36 C 0.27336(13) 0.46776(14) 0.11977(14) 0.0314(6) Uani 1 1 d . . . . .
C37 C 0.31028(16) 0.50565(16) 0.16817(16) 0.0465(9) Uani 1 1 d . . . . .
H37A H 0.285263 0.521966 0.199453 0.070 Uiso 1 1 calc R U . . .
H37B H 0.329156 0.542864 0.149005 0.070 Uiso 1 1 calc R U . . .
H37C H 0.340135 0.476455 0.187146 0.070 Uiso 1 1 calc R U . . .
C38 C 0.22535(15) 0.51275(16) 0.09235(17) 0.0467(8) Uani 1 1 d . . . . .
H38A H 0.201583 0.488697 0.061100 0.070 Uiso 1 1 calc R U . . .
H38B H 0.243013 0.551112 0.073757 0.070 Uiso 1 1 calc R U . . .
H38C H 0.200652 0.527310 0.124612 0.070 Uiso 1 1 calc R U . . .
C39 C 0.31245(17) 0.44506(17) 0.06938(17) 0.0514(9) Uani 1 1 d . . . . .
H39A H 0.342997 0.415906 0.087061 0.077 Uiso 1 1 calc R U . . .
H39B H 0.330438 0.483461 0.051197 0.077 Uiso 1 1 calc R U . . .
H39C H 0.288814 0.421353 0.037783 0.077 Uiso 1 1 calc R U . . .
C310 C 0.06420(12) 0.03615(13) 0.11093(13) 0.0275(6) Uani 1 1 d . . . . .
C311 C 0.0489(3) -0.0175(3) 0.1585(3) 0.0503(14) Uani 0.609(4) 1 d . . P A 1
H31A H 0.030053 -0.054915 0.137048 0.075 Uiso 0.609(4) 1 calc R U P A 1
H31B H 0.022286 0.001102 0.187138 0.075 Uiso 0.609(4) 1 calc R U P A 1
H31C H 0.084690 -0.032362 0.180941 0.075 Uiso 0.609(4) 1 calc R U P A 1
C312 C 0.0993(3) 0.0065(3) 0.0631(3) 0.0460(15) Uani 0.609(4) 1 d . . P A 1
H31D H 0.106942 0.039837 0.032333 0.069 Uiso 0.609(4) 1 calc R U P A 1
H31E H 0.077645 -0.030158 0.043586 0.069 Uiso 0.609(4) 1 calc R U P A 1
H31F H 0.136391 -0.009622 0.081942 0.069 Uiso 0.609(4) 1 calc R U P A 1
C313 C 0.0045(2) 0.0608(3) 0.0820(3) 0.0420(13) Uani 0.609(4) 1 d . . P A 1
H31G H 0.011211 0.092632 0.049598 0.063 Uiso 0.609(4) 1 calc R U P A 1
H31H H -0.017540 0.081846 0.113450 0.063 Uiso 0.609(4) 1 calc R U P A 1
H31I H -0.017755 0.023393 0.064585 0.063 Uiso 0.609(4) 1 calc R U P A 1
C31A C 0.0911(5) -0.0260(4) 0.1393(4) 0.0503(14) Uani 0.391(4) 1 d . . P A 2
H31J H 0.080448 -0.029842 0.181693 0.075 Uiso 0.391(4) 1 calc R U P A 2
H31K H 0.133672 -0.023859 0.138298 0.075 Uiso 0.391(4) 1 calc R U P A 2
H31L H 0.076565 -0.064463 0.116036 0.075 Uiso 0.391(4) 1 calc R U P A 2
C31B C 0.0781(4) 0.0365(5) 0.0406(5) 0.0460(15) Uani 0.391(4) 1 d . . P A 2
H31M H 0.061101 -0.002763 0.020552 0.069 Uiso 0.391(4) 1 calc R U P A 2
H31N H 0.120392 0.036418 0.037191 0.069 Uiso 0.391(4) 1 calc R U P A 2
H31O H 0.061208 0.075924 0.020876 0.069 Uiso 0.391(4) 1 calc R U P A 2
C31C C 0.0024(4) 0.0424(5) 0.1175(5) 0.0420(13) Uani 0.391(4) 1 d . . P A 2
H31P H -0.004987 0.045677 0.160924 0.063 Uiso 0.391(4) 1 calc R U P A 2
H31Q H -0.017775 0.003700 0.099831 0.063 Uiso 0.391(4) 1 calc R U P A 2
H31R H -0.012197 0.082016 0.096168 0.063 Uiso 0.391(4) 1 calc R U P A 2
C314 C 0.21686(14) 0.22449(16) 0.04404(14) 0.0386(7) Uani 1 1 d . . . . .
H31S H 0.229334 0.259948 0.017559 0.058 Uiso 1 1 calc R U . . .
H31T H 0.200194 0.188528 0.018841 0.058 Uiso 1 1 calc R U . . .
H31U H 0.250525 0.208229 0.069284 0.058 Uiso 1 1 calc R U . . .
C315 C 0.09678(14) 0.29143(15) 0.05334(15) 0.0403(8) Uani 1 1 d . . . . .
H31V H 0.069685 0.306521 0.083162 0.060 Uiso 1 1 calc R U . . .
H31W H 0.077661 0.258039 0.026818 0.060 Uiso 1 1 calc R U . . .
H31Z H 0.108311 0.328734 0.028511 0.060 Uiso 1 1 calc R U . . .
C316 C 0.26471(12) 0.19632(13) 0.28968(12) 0.0261(6) Uani 1 1 d . . . . .
C317 C 0.16593(13) 0.17792(14) 0.36119(13) 0.0335(7) Uani 1 1 d . . . . .
C318 C 0.22518(11) 0.30066(13) 0.36308(12) 0.0248(6) Uani 1 1 d . . . . .
C319 C 0.10906(12) 0.29015(14) 0.30733(13) 0.0298(6) Uani 1 1 d . . . . .
O31 O 0.30836(9) 0.17053(11) 0.28604(10) 0.0382(5) Uani 1 1 d . . . . .
O32 O 0.15451(12) 0.14094(12) 0.39818(11) 0.0536(6) Uani 1 1 d . . . . .
O33 O 0.24723(10) 0.33275(10) 0.40005(9) 0.0381(5) Uani 1 1 d . . . . .
O34 O 0.06597(10) 0.31643(13) 0.31347(11) 0.0522(6) Uani 1 1 d . . . . .
W4 W -0.11233(2) 0.25730(2) 0.45781(2) 0.02217(3) Uani 1 1 d . . . . .
P41 P -0.07061(3) 0.18258(3) 0.53408(3) 0.02445(14) Uani 1 1 d . . . . .
P42 P -0.12868(3) 0.33254(3) 0.54034(3) 0.01907(13) Uani 1 1 d . . . . .
Si4 Si -0.08326(3) 0.25486(3) 0.66171(3) 0.01948(14) Uani 1 1 d . . . . .
N41 N -0.04015(10) 0.13954(11) 0.64129(11) 0.0301(5) Uani 1 1 d . . . . .
N42 N -0.06530(9) 0.19258(10) 0.60974(10) 0.0240(5) Uani 1 1 d . . . . .
N43 N -0.12948(9) 0.36954(10) 0.65203(10) 0.0235(5) Uani 1 1 d . . . . .
N44 N -0.11381(9) 0.31828(10) 0.61494(9) 0.0193(4) Uani 1 1 d . . . . .
C42 C -0.04060(13) 0.10717(14) 0.53995(14) 0.0343(7) Uani 1 1 d . . . . .
H42 H -0.033931 0.078706 0.506761 0.041 Uiso 1 1 calc R U . . .
C43 C -0.02695(13) 0.09312(14) 0.60225(14) 0.0329(7) Uani 1 1 d . . . . .
C44 C -0.15568(11) 0.40747(12) 0.55475(12) 0.0225(5) Uani 1 1 d . . . . .
H44 H -0.170850 0.437759 0.524846 0.027 Uiso 1 1 calc R U . . .
C45 C -0.15214(11) 0.41799(12) 0.61842(12) 0.0237(5) Uani 1 1 d . . . . .
C46 C 0.00171(15) 0.02990(16) 0.62580(17) 0.0452(8) Uani 1 1 d . . . . .
C47 C 0.06357(15) 0.02656(18) 0.6044(2) 0.0627(12) Uani 1 1 d . . . . .
H47A H 0.062234 0.029863 0.559710 0.094 Uiso 1 1 calc R U . . .
H47B H 0.081534 -0.015308 0.617215 0.094 Uiso 1 1 calc R U . . .
H47C H 0.086673 0.062994 0.622369 0.094 Uiso 1 1 calc R U . . .
C48 C -0.03315(16) -0.02942(16) 0.6001(2) 0.0566(10) Uani 1 1 d . . . . .
H48A H -0.072807 -0.027861 0.614154 0.085 Uiso 1 1 calc R U . . .
H48B H -0.014033 -0.070139 0.614467 0.085 Uiso 1 1 calc R U . . .
H48C H -0.034873 -0.028110 0.555386 0.085 Uiso 1 1 calc R U . . .
C49 C 0.00159(19) 0.0260(2) 0.69524(19) 0.0641(11) Uani 1 1 d . . . . .
H49A H 0.026427 0.060904 0.713504 0.096 Uiso 1 1 calc R U . . .
H49B H 0.016595 -0.016895 0.709114 0.096 Uiso 1 1 calc R U . . .
H49C H -0.038337 0.031597 0.707729 0.096 Uiso 1 1 calc R U . . .
C410 C -0.17361(13) 0.47895(14) 0.65074(14) 0.0342(7) Uani 1 1 d . . . . .
C411 C -0.23885(13) 0.48591(17) 0.63766(16) 0.0456(9) Uani 1 1 d . . . . .
H41A H -0.247836 0.486577 0.593390 0.068 Uiso 1 1 calc R U . . .
H41B H -0.252155 0.526986 0.655558 0.068 Uiso 1 1 calc R U . . .
H41C H -0.258779 0.448655 0.655578 0.068 Uiso 1 1 calc R U . . .
C412 C -0.14391(19) 0.53936(17) 0.6252(3) 0.0829(16) Uani 1 1 d . . . . .
H41D H -0.153377 0.542267 0.581108 0.124 Uiso 1 1 calc R U . . .
H41E H -0.101569 0.535539 0.633007 0.124 Uiso 1 1 calc R U . . .
H41F H -0.157736 0.579017 0.645185 0.124 Uiso 1 1 calc R U . . .
C413 C -0.1589(2) 0.4734(2) 0.71930(18) 0.0804(16) Uani 1 1 d . . . . .
H41G H -0.170953 0.513690 0.739545 0.121 Uiso 1 1 calc R U . . .
H41H H -0.116739 0.467296 0.726920 0.121 Uiso 1 1 calc R U . . .
H41I H -0.179493 0.435683 0.735517 0.121 Uiso 1 1 calc R U . . .
C414 C -0.01599(13) 0.28456(16) 0.70150(15) 0.0384(7) Uani 1 1 d . . . . .
H41J H 0.011808 0.297285 0.671487 0.058 Uiso 1 1 calc R U . . .
H41K H 0.000994 0.249584 0.727700 0.058 Uiso 1 1 calc R U . . .
H41L H -0.024717 0.322737 0.726623 0.058 Uiso 1 1 calc R U . . .
C415 C -0.13853(14) 0.22539(15) 0.71174(14) 0.0348(7) Uani 1 1 d . . . . .
H41M H -0.150140 0.261398 0.738081 0.052 Uiso 1 1 calc R U . . .
H41N H -0.122379 0.189265 0.737082 0.052 Uiso 1 1 calc R U . . .
H41O H -0.172657 0.209727 0.686859 0.052 Uiso 1 1 calc R U . . .
C416 C -0.03371(13) 0.30190(16) 0.44719(13) 0.0348(7) Uani 1 1 d . . . . .
C417 C -0.15205(13) 0.31836(15) 0.39640(13) 0.0317(6) Uani 1 1 d . . . . .
C418 C -0.09414(14) 0.19393(16) 0.39102(14) 0.0366(7) Uani 1 1 d . . . . .
C419 C -0.19094(13) 0.21208(14) 0.46648(12) 0.0272(6) Uani 1 1 d . . . . .
O41 O 0.00978(10) 0.32683(14) 0.44029(12) 0.0563(7) Uani 1 1 d . . . . .
O42 O -0.17580(11) 0.35212(12) 0.36155(10) 0.0510(6) Uani 1 1 d . . . . .
O43 O -0.08317(12) 0.15828(13) 0.35311(11) 0.0566(7) Uani 1 1 d . . . . .
O44 O -0.23474(9) 0.18621(10) 0.47022(10) 0.0378(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C117 2.010(3) . ?
W1 C118 2.011(3) . ?
W1 C116 2.040(3) . ?
W1 C119 2.047(3) . ?
W1 P12 2.4103(6) . ?
W1 P11 2.4151(6) . ?
P11 N12 1.674(2) . ?
P11 C12 1.683(3) . ?
P12 N14 1.666(2) . ?
P12 C15 1.689(2) . ?
Si1 N12 1.771(2) . ?
Si1 N14 1.777(2) . ?
Si1 C115 1.828(3) . ?
Si1 C114 1.835(3) . ?
N11 C13 1.322(3) . ?
N11 N12 1.391(3) . ?
N13 C14 1.322(3) . ?
N13 N14 1.384(3) . ?
C12 C13 1.416(3) . ?
C12 H12 0.9500 . ?
C13 C16 1.520(3) . ?
C14 C15 1.410(3) . ?
C14 C110 1.525(3) . ?
C15 H15 0.9500 . ?
C16 C19 1.499(5) . ?
C16 C17 1.516(4) . ?
C16 C18 1.522(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C110 C113 1.523(4) . ?
C110 C111 1.532(4) . ?
C110 C112 1.533(4) . ?
C111 H11A 0.9800 . ?
C111 H11B 0.9800 . ?
C111 H11C 0.9800 . ?
C112 H11D 0.9800 . ?
C112 H11E 0.9800 . ?
C112 H11F 0.9800 . ?
C113 H11G 0.9800 . ?
C113 H11H 0.9800 . ?
C113 H11I 0.9800 . ?
C114 H11J 0.9800 . ?
C114 H11K 0.9800 . ?
C114 H11L 0.9800 . ?
C115 H11M 0.9800 . ?
C115 H11N 0.9800 . ?
C115 H11O 0.9800 . ?
C116 O11 1.142(3) . ?
C117 O12 1.142(3) . ?
C118 O13 1.139(3) . ?
C119 O14 1.140(3) . ?
W2 C218 2.010(3) . ?
W2 C217 2.013(3) . ?
W2 C219 2.046(3) . ?
W2 C216 2.049(3) . ?
W2 P21 2.4037(6) . ?
W2 P22 2.4129(6) . ?
P21 N22 1.668(2) . ?
P21 C22 1.682(3) . ?
P22 N24 1.671(2) . ?
P22 C25 1.684(2) . ?
Si2 N22 1.774(2) . ?
Si2 N24 1.774(2) . ?
Si2 C215 1.825(3) . ?
Si2 C214 1.830(3) . ?
N21 C23 1.325(3) . ?
N21 N22 1.383(3) . ?
N23 C24 1.326(3) . ?
N23 N24 1.385(3) . ?
C22 C23 1.409(3) . ?
C22 H22 0.9500 . ?
C23 C26 1.519(3) . ?
C24 C25 1.409(3) . ?
C24 C210 1.520(3) . ?
C25 H25 0.9500 . ?
C26 C28 1.530(4) . ?
C26 C27 1.532(4) . ?
C26 C29 1.533(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C210 C212 1.526(4) . ?
C210 C211 1.530(4) . ?
C210 C213 1.536(4) . ?
C211 H21A 0.9800 . ?
C211 H21B 0.9800 . ?
C211 H21C 0.9800 . ?
C212 H21D 0.9800 . ?
C212 H21E 0.9800 . ?
C212 H21F 0.9800 . ?
C213 H21G 0.9800 . ?
C213 H21H 0.9800 . ?
C213 H21I 0.9800 . ?
C214 H21J 0.9800 . ?
C214 H21K 0.9800 . ?
C214 H21L 0.9800 . ?
C215 H21M 0.9800 . ?
C215 H21N 0.9800 . ?
C215 H21O 0.9800 . ?
C216 O21 1.138(3) . ?
C217 O22 1.140(3) . ?
C218 O23 1.141(3) . ?
C219 O24 1.141(3) . ?
W3 C317 2.008(3) . ?
W3 C318 2.014(3) . ?
W3 C316 2.046(3) . ?
W3 C319 2.047(3) . ?
W3 P32 2.4159(6) . ?
W3 P31 2.4179(7) . ?
P31 N32 1.673(2) . ?
P31 C32 1.687(3) . ?
P32 N34 1.673(2) . ?
P32 C35 1.687(3) . ?
Si3 N32 1.771(2) . ?
Si3 N34 1.772(2) . ?
Si3 C315 1.832(3) . ?
Si3 C314 1.836(3) . ?
N31 C33 1.325(3) . ?
N31 N32 1.386(3) . ?
N33 C34 1.318(3) . ?
N33 N34 1.388(3) . ?
C32 C33 1.411(4) . ?
C32 H32 0.9500 . ?
C33 C36 1.524(4) . ?
C34 C35 1.414(4) . ?
C34 C310 1.523(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.526(4) . ?
C36 C38 1.527(4) . ?
C36 C39 1.538(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C310 C31C 1.443(10) . ?
C310 C312 1.490(6) . ?
C310 C31A 1.523(10) . ?
C310 C313 1.558(6) . ?
C310 C311 1.564(6) . ?
C310 C31B 1.594(11) . ?
C311 H31A 0.9800 . ?
C311 H31B 0.9800 . ?
C311 H31C 0.9800 . ?
C312 H31D 0.9800 . ?
C312 H31E 0.9800 . ?
C312 H31F 0.9800 . ?
C313 H31G 0.9800 . ?
C313 H31H 0.9800 . ?
C313 H31I 0.9800 . ?
C31A H31J 0.9800 . ?
C31A H31K 0.9800 . ?
C31A H31L 0.9800 . ?
C31B H31M 0.9800 . ?
C31B H31N 0.9800 . ?
C31B H31O 0.9800 . ?
C31C H31P 0.9800 . ?
C31C H31Q 0.9800 . ?
C31C H31R 0.9800 . ?
C314 H31S 0.9800 . ?
C314 H31T 0.9800 . ?
C314 H31U 0.9800 . ?
C315 H31V 0.9800 . ?
C315 H31W 0.9800 . ?
C315 H31Z 0.9800 . ?
C316 O31 1.139(3) . ?
C317 O32 1.148(4) . ?
C318 O33 1.135(3) . ?
C319 O34 1.140(3) . ?
W4 C417 2.009(3) . ?
W4 C418 2.014(3) . ?
W4 C419 2.046(3) . ?
W4 C416 2.047(3) . ?
W4 P41 2.4136(7) . ?
W4 P42 2.4175(6) . ?
P41 N42 1.669(2) . ?
P41 C42 1.683(3) . ?
P42 N44 1.676(2) . ?
P42 C44 1.683(3) . ?
Si4 N44 1.766(2) . ?
Si4 N42 1.770(2) . ?
Si4 C414 1.829(3) . ?
Si4 C415 1.830(3) . ?
N41 C43 1.322(4) . ?
N41 N42 1.388(3) . ?
N43 C45 1.318(3) . ?
N43 N44 1.384(3) . ?
C42 C43 1.412(4) . ?
C42 H42 0.9500 . ?
C43 C46 1.520(4) . ?
C44 C45 1.410(4) . ?
C44 H44 0.9500 . ?
C45 C410 1.525(4) . ?
C46 C49 1.525(5) . ?
C46 C47 1.526(5) . ?
C46 C48 1.535(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C410 C411 1.515(4) . ?
C410 C413 1.525(5) . ?
C410 C412 1.528(5) . ?
C411 H41A 0.9800 . ?
C411 H41B 0.9800 . ?
C411 H41C 0.9800 . ?
C412 H41D 0.9800 . ?
C412 H41E 0.9800 . ?
C412 H41F 0.9800 . ?
C413 H41G 0.9800 . ?
C413 H41H 0.9800 . ?
C413 H41I 0.9800 . ?
C414 H41J 0.9800 . ?
C414 H41K 0.9800 . ?
C414 H41L 0.9800 . ?
C415 H41M 0.9800 . ?
C415 H41N 0.9800 . ?
C415 H41O 0.9800 . ?
C416 O41 1.139(4) . ?
C417 O42 1.141(3) . ?
C418 O43 1.143(4) . ?
C419 O44 1.143(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C117 W1 C118 88.82(11) . . ?
C117 W1 C116 91.76(11) . . ?
C118 W1 C116 90.72(11) . . ?
C117 W1 C119 91.42(11) . . ?
C118 W1 C119 90.78(11) . . ?
C116 W1 C119 176.51(10) . . ?
C117 W1 P12 89.89(8) . . ?
C118 W1 P12 178.59(8) . . ?
C116 W1 P12 88.76(7) . . ?
C119 W1 P12 89.81(7) . . ?
C117 W1 P11 178.17(8) . . ?
C118 W1 P11 93.01(8) . . ?
C116 W1 P11 88.23(8) . . ?
C119 W1 P11 88.55(7) . . ?
P12 W1 P11 88.28(2) . . ?
N12 P11 C12 91.76(11) . . ?
N12 P11 W1 126.30(7) . . ?
C12 P11 W1 141.94(9) . . ?
N14 P12 C15 91.71(11) . . ?
N14 P12 W1 126.82(7) . . ?
C15 P12 W1 141.44(9) . . ?
N12 Si1 N14 105.31(9) . . ?
N12 Si1 C115 110.13(12) . . ?
N14 Si1 C115 109.01(12) . . ?
N12 Si1 C114 108.41(12) . . ?
N14 Si1 C114 108.95(11) . . ?
C115 Si1 C114 114.62(14) . . ?
C13 N11 N12 110.14(19) . . ?
N11 N12 P11 113.46(15) . . ?
N11 N12 Si1 109.77(15) . . ?
P11 N12 Si1 136.48(12) . . ?
C14 N13 N14 109.98(19) . . ?
N13 N14 P12 113.80(15) . . ?
N13 N14 Si1 109.93(15) . . ?
P12 N14 Si1 136.12(12) . . ?
C13 C12 P11 109.15(18) . . ?
C13 C12 H12 125.4 . . ?
P11 C12 H12 125.4 . . ?
N11 C13 C12 115.5(2) . . ?
N11 C13 C16 119.6(2) . . ?
C12 C13 C16 124.9(2) . . ?
N13 C14 C15 115.8(2) . . ?
N13 C14 C110 117.6(2) . . ?
C15 C14 C110 126.6(2) . . ?
C14 C15 P12 108.70(18) . . ?
C14 C15 H15 125.6 . . ?
P12 C15 H15 125.6 . . ?
C19 C16 C17 109.7(3) . . ?
C19 C16 C13 110.8(2) . . ?
C17 C16 C13 109.6(2) . . ?
C19 C16 C18 111.4(3) . . ?
C17 C16 C18 106.9(3) . . ?
C13 C16 C18 108.4(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C113 C110 C14 110.9(2) . . ?
C113 C110 C111 109.8(2) . . ?
C14 C110 C111 108.6(2) . . ?
C113 C110 C112 109.4(2) . . ?
C14 C110 C112 109.3(2) . . ?
C111 C110 C112 108.7(2) . . ?
C110 C111 H11A 109.5 . . ?
C110 C111 H11B 109.5 . . ?
H11A C111 H11B 109.5 . . ?
C110 C111 H11C 109.5 . . ?
H11A C111 H11C 109.5 . . ?
H11B C111 H11C 109.5 . . ?
C110 C112 H11D 109.5 . . ?
C110 C112 H11E 109.5 . . ?
H11D C112 H11E 109.5 . . ?
C110 C112 H11F 109.5 . . ?
H11D C112 H11F 109.5 . . ?
H11E C112 H11F 109.5 . . ?
C110 C113 H11G 109.5 . . ?
C110 C113 H11H 109.5 . . ?
H11G C113 H11H 109.5 . . ?
C110 C113 H11I 109.5 . . ?
H11G C113 H11I 109.5 . . ?
H11H C113 H11I 109.5 . . ?
Si1 C114 H11J 109.5 . . ?
Si1 C114 H11K 109.5 . . ?
H11J C114 H11K 109.5 . . ?
Si1 C114 H11L 109.5 . . ?
H11J C114 H11L 109.5 . . ?
H11K C114 H11L 109.5 . . ?
Si1 C115 H11M 109.5 . . ?
Si1 C115 H11N 109.5 . . ?
H11M C115 H11N 109.5 . . ?
Si1 C115 H11O 109.5 . . ?
H11M C115 H11O 109.5 . . ?
H11N C115 H11O 109.5 . . ?
O11 C116 W1 178.1(2) . . ?
O12 C117 W1 179.6(3) . . ?
O13 C118 W1 178.3(2) . . ?
O14 C119 W1 178.7(2) . . ?
C218 W2 C217 89.40(11) . . ?
C218 W2 C219 91.53(12) . . ?
C217 W2 C219 90.98(11) . . ?
C218 W2 C216 90.52(12) . . ?
C217 W2 C216 91.40(11) . . ?
C219 W2 C216 176.87(10) . . ?
C218 W2 P21 90.45(8) . . ?
C217 W2 P21 178.57(8) . . ?
C219 W2 P21 87.60(8) . . ?
C216 W2 P21 90.02(7) . . ?
C218 W2 P22 178.37(9) . . ?
C217 W2 P22 91.98(8) . . ?
C219 W2 P22 89.30(8) . . ?
C216 W2 P22 88.59(8) . . ?
P21 W2 P22 88.19(2) . . ?
N22 P21 C22 91.74(11) . . ?
N22 P21 W2 126.91(7) . . ?
C22 P21 W2 141.33(9) . . ?
N24 P22 C25 91.63(11) . . ?
N24 P22 W2 126.48(7) . . ?
C25 P22 W2 141.86(9) . . ?
N22 Si2 N24 105.27(9) . . ?
N22 Si2 C215 108.36(12) . . ?
N24 Si2 C215 109.67(12) . . ?
N22 Si2 C214 109.32(12) . . ?
N24 Si2 C214 108.36(12) . . ?
C215 Si2 C214 115.39(15) . . ?
C23 N21 N22 109.86(19) . . ?
N21 N22 P21 113.77(15) . . ?
N21 N22 Si2 109.77(15) . . ?
P21 N22 Si2 136.41(12) . . ?
C24 N23 N24 109.87(19) . . ?
N23 N24 P22 113.77(15) . . ?
N23 N24 Si2 109.62(15) . . ?
P22 N24 Si2 136.53(12) . . ?
C23 C22 P21 108.98(18) . . ?
C23 C22 H22 125.5 . . ?
P21 C22 H22 125.5 . . ?
N21 C23 C22 115.7(2) . . ?
N21 C23 C26 117.9(2) . . ?
C22 C23 C26 126.4(2) . . ?
N23 C24 C25 115.6(2) . . ?
N23 C24 C210 118.0(2) . . ?
C25 C24 C210 126.4(2) . . ?
C24 C25 P22 109.16(18) . . ?
C24 C25 H25 125.4 . . ?
P22 C25 H25 125.4 . . ?
C23 C26 C28 107.6(2) . . ?
C23 C26 C27 110.6(2) . . ?
C28 C26 C27 109.5(2) . . ?
C23 C26 C29 110.2(2) . . ?
C28 C26 C29 109.7(2) . . ?
C27 C26 C29 109.1(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C24 C210 C212 109.1(2) . . ?
C24 C210 C211 110.6(2) . . ?
C212 C210 C211 109.0(2) . . ?
C24 C210 C213 109.1(2) . . ?
C212 C210 C213 110.4(2) . . ?
C211 C210 C213 108.6(2) . . ?
C210 C211 H21A 109.5 . . ?
C210 C211 H21B 109.5 . . ?
H21A C211 H21B 109.5 . . ?
C210 C211 H21C 109.5 . . ?
H21A C211 H21C 109.5 . . ?
H21B C211 H21C 109.5 . . ?
C210 C212 H21D 109.5 . . ?
C210 C212 H21E 109.5 . . ?
H21D C212 H21E 109.5 . . ?
C210 C212 H21F 109.5 . . ?
H21D C212 H21F 109.5 . . ?
H21E C212 H21F 109.5 . . ?
C210 C213 H21G 109.5 . . ?
C210 C213 H21H 109.5 . . ?
H21G C213 H21H 109.5 . . ?
C210 C213 H21I 109.5 . . ?
H21G C213 H21I 109.5 . . ?
H21H C213 H21I 109.5 . . ?
Si2 C214 H21J 109.5 . . ?
Si2 C214 H21K 109.5 . . ?
H21J C214 H21K 109.5 . . ?
Si2 C214 H21L 109.5 . . ?
H21J C214 H21L 109.5 . . ?
H21K C214 H21L 109.5 . . ?
Si2 C215 H21M 109.5 . . ?
Si2 C215 H21N 109.5 . . ?
H21M C215 H21N 109.5 . . ?
Si2 C215 H21O 109.5 . . ?
H21M C215 H21O 109.5 . . ?
H21N C215 H21O 109.5 . . ?
O21 C216 W2 178.7(2) . . ?
O22 C217 W2 178.7(3) . . ?
O23 C218 W2 179.7(3) . . ?
O24 C219 W2 178.1(2) . . ?
C317 W3 C318 89.92(11) . . ?
C317 W3 C316 89.84(12) . . ?
C318 W3 C316 89.02(10) . . ?
C317 W3 C319 89.27(12) . . ?
C318 W3 C319 90.00(11) . . ?
C316 W3 C319 178.68(11) . . ?
C317 W3 P32 91.53(8) . . ?
C318 W3 P32 177.93(8) . . ?
C316 W3 P32 89.52(7) . . ?
C319 W3 P32 91.48(8) . . ?
C317 W3 P31 178.95(9) . . ?
C318 W3 P31 91.04(8) . . ?
C316 W3 P31 90.60(8) . . ?
C319 W3 P31 90.31(9) . . ?
P32 W3 P31 87.52(2) . . ?
N32 P31 C32 91.73(12) . . ?
N32 P31 W3 127.18(8) . . ?
C32 P31 W3 141.01(10) . . ?
N34 P32 C35 91.85(12) . . ?
N34 P32 W3 126.72(8) . . ?
C35 P32 W3 141.42(10) . . ?
N32 Si3 N34 104.61(10) . . ?
N32 Si3 C315 109.78(13) . . ?
N34 Si3 C315 108.66(13) . . ?
N32 Si3 C314 108.72(13) . . ?
N34 Si3 C314 109.52(13) . . ?
C315 Si3 C314 115.05(16) . . ?
C33 N31 N32 110.1(2) . . ?
N31 N32 P31 113.56(16) . . ?
N31 N32 Si3 109.56(16) . . ?
P31 N32 Si3 136.65(13) . . ?
C34 N33 N34 110.2(2) . . ?
N33 N34 P32 113.40(17) . . ?
N33 N34 Si3 109.31(16) . . ?
P32 N34 Si3 137.26(13) . . ?
C33 C32 P31 109.00(19) . . ?
C33 C32 H32 125.5 . . ?
P31 C32 H32 125.5 . . ?
N31 C33 C32 115.6(2) . . ?
N31 C33 C36 118.1(2) . . ?
C32 C33 C36 126.3(2) . . ?
N33 C34 C35 115.8(2) . . ?
N33 C34 C310 118.1(2) . . ?
C35 C34 C310 126.0(2) . . ?
C34 C35 P32 108.7(2) . . ?
C34 C35 H35 125.6 . . ?
P32 C35 H35 125.6 . . ?
C33 C36 C37 110.6(2) . . ?
C33 C36 C38 108.8(2) . . ?
C37 C36 C38 109.1(3) . . ?
C33 C36 C39 109.5(2) . . ?
C37 C36 C39 109.1(3) . . ?
C38 C36 C39 109.7(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C31C C310 C34 109.8(4) . . ?
C312 C310 C34 110.8(3) . . ?
C31C C310 C31A 114.2(6) . . ?
C34 C310 C31A 107.1(4) . . ?
C312 C310 C313 110.1(4) . . ?
C34 C310 C313 108.5(3) . . ?
C312 C310 C311 109.9(4) . . ?
C34 C310 C311 111.8(3) . . ?
C313 C310 C311 105.5(4) . . ?
C31C C310 C31B 110.7(6) . . ?
C34 C310 C31B 107.5(4) . . ?
C31A C310 C31B 107.3(6) . . ?
C310 C311 H31A 109.5 . . ?
C310 C311 H31B 109.5 . . ?
H31A C311 H31B 109.5 . . ?
C310 C311 H31C 109.5 . . ?
H31A C311 H31C 109.5 . . ?
H31B C311 H31C 109.5 . . ?
C310 C312 H31D 109.5 . . ?
C310 C312 H31E 109.5 . . ?
H31D C312 H31E 109.5 . . ?
C310 C312 H31F 109.5 . . ?
H31D C312 H31F 109.5 . . ?
H31E C312 H31F 109.5 . . ?
C310 C313 H31G 109.5 . . ?
C310 C313 H31H 109.5 . . ?
H31G C313 H31H 109.5 . . ?
C310 C313 H31I 109.5 . . ?
H31G C313 H31I 109.5 . . ?
H31H C313 H31I 109.5 . . ?
C310 C31A H31J 109.5 . . ?
C310 C31A H31K 109.5 . . ?
H31J C31A H31K 109.5 . . ?
C310 C31A H31L 109.5 . . ?
H31J C31A H31L 109.5 . . ?
H31K C31A H31L 109.5 . . ?
C310 C31B H31M 109.5 . . ?
C310 C31B H31N 109.5 . . ?
H31M C31B H31N 109.5 . . ?
C310 C31B H31O 109.5 . . ?
H31M C31B H31O 109.5 . . ?
H31N C31B H31O 109.5 . . ?
C310 C31C H31P 109.5 . . ?
C310 C31C H31Q 109.5 . . ?
H31P C31C H31Q 109.5 . . ?
C310 C31C H31R 109.5 . . ?
H31P C31C H31R 109.5 . . ?
H31Q C31C H31R 109.5 . . ?
Si3 C314 H31S 109.5 . . ?
Si3 C314 H31T 109.5 . . ?
H31S C314 H31T 109.5 . . ?
Si3 C314 H31U 109.5 . . ?
H31S C314 H31U 109.5 . . ?
H31T C314 H31U 109.5 . . ?
Si3 C315 H31V 109.5 . . ?
Si3 C315 H31W 109.5 . . ?
H31V C315 H31W 109.5 . . ?
Si3 C315 H31Z 109.5 . . ?
H31V C315 H31Z 109.5 . . ?
H31W C315 H31Z 109.5 . . ?
O31 C316 W3 179.1(3) . . ?
O32 C317 W3 179.1(3) . . ?
O33 C318 W3 179.5(3) . . ?
O34 C319 W3 179.3(3) . . ?
C417 W4 C418 90.82(12) . . ?
C417 W4 C419 88.49(11) . . ?
C418 W4 C419 90.26(12) . . ?
C417 W4 C416 90.96(12) . . ?
C418 W4 C416 88.64(13) . . ?
C419 W4 C416 178.76(11) . . ?
C417 W4 P41 176.34(9) . . ?
C418 W4 P41 90.55(9) . . ?
C419 W4 P41 88.11(8) . . ?
C416 W4 P41 92.47(9) . . ?
C417 W4 P42 91.45(8) . . ?
C418 W4 P42 176.82(9) . . ?
C419 W4 P42 92.03(8) . . ?
C416 W4 P42 89.10(8) . . ?
P41 W4 P42 87.31(2) . . ?
N42 P41 C42 91.77(13) . . ?
N42 P41 W4 127.85(8) . . ?
C42 P41 W4 140.33(11) . . ?
N44 P42 C44 91.63(12) . . ?
N44 P42 W4 126.14(8) . . ?
C44 P42 W4 142.21(10) . . ?
N44 Si4 N42 104.41(10) . . ?
N44 Si4 C414 109.21(12) . . ?
N42 Si4 C414 108.63(13) . . ?
N44 Si4 C415 108.79(13) . . ?
N42 Si4 C415 110.50(13) . . ?
C414 Si4 C415 114.78(15) . . ?
C43 N41 N42 109.7(2) . . ?
N41 N42 P41 113.77(17) . . ?
N41 N42 Si4 109.99(17) . . ?
P41 N42 Si4 136.24(13) . . ?
C45 N43 N44 110.0(2) . . ?
N43 N44 P42 113.51(16) . . ?
N43 N44 Si4 108.50(15) . . ?
P42 N44 Si4 137.98(13) . . ?
C43 C42 P41 108.9(2) . . ?
C43 C42 H42 125.6 . . ?
P41 C42 H42 125.6 . . ?
N41 C43 C42 115.9(2) . . ?
N41 C43 C46 119.7(3) . . ?
C42 C43 C46 124.4(3) . . ?
C45 C44 P42 108.92(19) . . ?
C45 C44 H44 125.5 . . ?
P42 C44 H44 125.5 . . ?
N43 C45 C44 115.9(2) . . ?
N43 C45 C410 118.4(2) . . ?
C44 C45 C410 125.7(2) . . ?
C43 C46 C49 110.8(3) . . ?
C43 C46 C47 108.9(3) . . ?
C49 C46 C47 111.4(3) . . ?
C43 C46 C48 109.6(3) . . ?
C49 C46 C48 107.0(3) . . ?
C47 C46 C48 109.1(3) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C411 C410 C413 110.5(3) . . ?
C411 C410 C45 109.4(2) . . ?
C413 C410 C45 109.9(3) . . ?
C411 C410 C412 108.3(3) . . ?
C413 C410 C412 110.1(4) . . ?
C45 C410 C412 108.6(3) . . ?
C410 C411 H41A 109.5 . . ?
C410 C411 H41B 109.5 . . ?
H41A C411 H41B 109.5 . . ?
C410 C411 H41C 109.5 . . ?
H41A C411 H41C 109.5 . . ?
H41B C411 H41C 109.5 . . ?
C410 C412 H41D 109.5 . . ?
C410 C412 H41E 109.5 . . ?
H41D C412 H41E 109.5 . . ?
C410 C412 H41F 109.5 . . ?
H41D C412 H41F 109.5 . . ?
H41E C412 H41F 109.5 . . ?
C410 C413 H41G 109.5 . . ?
C410 C413 H41H 109.5 . . ?
H41G C413 H41H 109.5 . . ?
C410 C413 H41I 109.5 . . ?
H41G C413 H41I 109.5 . . ?
H41H C413 H41I 109.5 . . ?
Si4 C414 H41J 109.5 . . ?
Si4 C414 H41K 109.5 . . ?
H41J C414 H41K 109.5 . . ?
Si4 C414 H41L 109.5 . . ?
H41J C414 H41L 109.5 . . ?
H41K C414 H41L 109.5 . . ?
Si4 C415 H41M 109.5 . . ?
Si4 C415 H41N 109.5 . . ?
H41M C415 H41N 109.5 . . ?
Si4 C415 H41O 109.5 . . ?
H41M C415 H41O 109.5 . . ?
H41N C415 H41O 109.5 . . ?
O41 C416 W4 178.9(3) . . ?
O42 C417 W4 178.3(3) . . ?
O43 C418 W4 179.2(3) . . ?
O44 C419 W4 178.6(2) . . ?

_refine_diff_density_max         1.227
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.108

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me190204Cr1_14
_database_code_depnum_ccdc_archive 'CCDC 1920919'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 Cr N4 O4 P2 Si'
_chemical_formula_sum            'C16 H22 Cr N4 O4 P2 Si'
_chemical_formula_weight         476.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8157(3)
_cell_length_b                   9.8348(4)
_cell_length_c                   25.7942(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.130(2)
_cell_angle_gamma                90
_cell_volume                     2213.90(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    46690
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.156
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.838
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            46690
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.571
_diffrn_reflns_theta_max         27.563
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5094
_reflns_number_gt                4245
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0286P)²+1.6763P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5094
_refine_ls_number_parameters     253
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0761
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.27369(3) 0.52070(3) 0.31417(2) 0.01674(8) Uani 1 1 d . U . . .
P1 P 0.11462(5) 0.60858(5) 0.36871(2) 0.01751(11) Uani 1 1 d . U . . .
Si1 Si 0.29687(6) 0.85896(5) 0.42439(2) 0.01772(12) Uani 1 1 d . U . . .
O1 O 0.11119(18) 0.25093(15) 0.31038(6) 0.0329(4) Uani 1 1 d . U . . .
N1 N 0.14375(18) 0.74342(17) 0.40835(6) 0.0196(3) Uani 1 1 d . U . . .
C2 C -0.0580(2) 0.5758(2) 0.38801(8) 0.0196(4) Uani 1 1 d . U . . .
O2 O 0.4634(2) 0.41427(18) 0.23465(7) 0.0500(5) Uani 1 1 d . U . . .
P2 P 0.42306(5) 0.71341(5) 0.32833(2) 0.01825(11) Uani 1 1 d . U . . .
N2 N 0.02598(18) 0.76709(17) 0.43751(6) 0.0216(4) Uani 1 1 d . U . . .
C1 C -0.0824(2) 0.6747(2) 0.42589(7) 0.0192(4) Uani 1 1 d . U . . .
O4 O 0.0580(2) 0.62644(17) 0.21962(6) 0.0412(4) Uani 1 1 d . U . . .
N3 N 0.41650(17) 0.82709(16) 0.37638(6) 0.0187(3) Uani 1 1 d . U . . .
C5 C -0.1669(2) 0.4639(2) 0.36893(10) 0.0320(5) Uani 1 1 d . U . . .
H5A H -0.1235 0.4094 0.3428 0.048 Uiso 1 1 calc R U . . .
H5B H -0.2647 0.5031 0.3530 0.048 Uiso 1 1 calc R U . . .
H5C H -0.1839 0.4059 0.3985 0.048 Uiso 1 1 calc R U . . .
O3 O 0.48113(19) 0.3883(2) 0.40388(7) 0.0494(5) Uani 1 1 d . U . . .
N4 N 0.53889(18) 0.91727(17) 0.38248(6) 0.0204(3) Uani 1 1 d . U . . .
C3 C -0.2197(2) 0.6798(2) 0.45430(8) 0.0248(4) Uani 1 1 d . U . . .
H3A H -0.3114 0.6502 0.4303 0.030 Uiso 1 1 calc R U . . .
H3B H -0.2367 0.7748 0.4648 0.030 Uiso 1 1 calc R U . . .
C4 C -0.2006(3) 0.5900(3) 0.50261(11) 0.0568(9) Uani 1 1 d . U . . .
H4A H -0.2925 0.5963 0.5199 0.085 Uiso 1 1 calc R U . . .
H4B H -0.1111 0.6201 0.5268 0.085 Uiso 1 1 calc R U . . .
H4C H -0.1859 0.4955 0.4923 0.085 Uiso 1 1 calc R U . . .
C7 C 0.5916(2) 0.7772(2) 0.31425(7) 0.0197(4) Uani 1 1 d . U . . .
C6 C 0.6318(2) 0.8884(2) 0.34815(8) 0.0201(4) Uani 1 1 d . U . . .
C10 C 0.6854(2) 0.7295(2) 0.27345(8) 0.0286(5) Uani 1 1 d . U . . .
H10A H 0.6352 0.6511 0.2549 0.043 Uiso 1 1 calc R U . . .
H10B H 0.7877 0.7032 0.2904 0.043 Uiso 1 1 calc R U . . .
H10C H 0.6944 0.8032 0.2485 0.043 Uiso 1 1 calc R U . . .
C8 C 0.7727(2) 0.9740(2) 0.34649(9) 0.0271(5) Uani 1 1 d . U . . .
H8A H 0.7670 1.0153 0.3113 0.033 Uiso 1 1 calc R U . . .
H8B H 0.8638 0.9140 0.3516 0.033 Uiso 1 1 calc R U . . .
C9 C 0.7948(3) 1.0861(2) 0.38692(11) 0.0423(6) Uani 1 1 d . U . . .
H9A H 0.8887 1.1366 0.3834 0.064 Uiso 1 1 calc R U . . .
H9B H 0.8032 1.0464 0.4221 0.064 Uiso 1 1 calc R U . . .
H9C H 0.7069 1.1480 0.3815 0.064 Uiso 1 1 calc R U . . .
C12 C 0.2252(2) 1.0342(2) 0.41809(10) 0.0324(5) Uani 1 1 d . U . . .
H12A H 0.1588 1.0515 0.4448 0.049 Uiso 1 1 calc R U . . .
H12B H 0.1666 1.0471 0.3832 0.049 Uiso 1 1 calc R U . . .
H12C H 0.3118 1.0976 0.4229 0.049 Uiso 1 1 calc R U . . .
C11 C 0.4006(3) 0.8141(3) 0.48907(8) 0.0328(5) Uani 1 1 d . U . . .
H11A H 0.3350 0.8316 0.5160 0.049 Uiso 1 1 calc R U . . .
H11B H 0.4938 0.8693 0.4962 0.049 Uiso 1 1 calc R U . . .
H11C H 0.4283 0.7176 0.4895 0.049 Uiso 1 1 calc R U . . .
C13 C 0.1686(2) 0.3559(2) 0.31069(8) 0.0221(4) Uani 1 1 d . U . . .
C14 C 0.3947(3) 0.4556(2) 0.26575(9) 0.0286(5) Uani 1 1 d . U . . .
C16 C 0.1383(2) 0.5906(2) 0.25536(8) 0.0242(4) Uani 1 1 d . U . . .
C15 C 0.4044(2) 0.4408(2) 0.37059(8) 0.0270(5) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 C13 1.863(2) . ?
Cr1 C14 1.866(2) . ?
Cr1 C15 1.894(2) . ?
Cr1 C16 1.920(2) . ?
Cr1 P1 2.2916(5) . ?
Cr1 P2 2.3072(6) . ?
P1 N1 1.6721(17) . ?
P1 C2 1.6978(18) . ?
Si1 N3 1.7645(16) . ?
Si1 N1 1.7682(17) . ?
Si1 C12 1.835(2) . ?
Si1 C11 1.839(2) . ?
O1 C13 1.149(2) . ?
N1 N2 1.385(2) . ?
C2 C1 1.416(3) . ?
C2 C5 1.497(3) . ?
O2 C14 1.146(2) . ?
P2 N3 1.6762(16) . ?
P2 C7 1.6987(19) . ?
N2 C1 1.322(3) . ?
C1 C3 1.502(2) . ?
O4 C16 1.136(3) . ?
N3 N4 1.388(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O3 C15 1.139(3) . ?
N4 C6 1.319(2) . ?
C3 C4 1.517(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C7 C6 1.414(3) . ?
C7 C10 1.502(3) . ?
C6 C8 1.507(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8 C9 1.511(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Cr1 C14 89.80(9) . . ?
C13 Cr1 C15 85.43(9) . . ?
C14 Cr1 C15 91.65(9) . . ?
C13 Cr1 C16 91.39(9) . . ?
C14 Cr1 C16 86.81(9) . . ?
C15 Cr1 C16 176.48(9) . . ?
C13 Cr1 P1 90.83(6) . . ?
C14 Cr1 P1 175.86(7) . . ?
C15 Cr1 P1 92.48(6) . . ?
C16 Cr1 P1 89.08(6) . . ?
C13 Cr1 P2 172.39(7) . . ?
C14 Cr1 P2 91.17(7) . . ?
C15 Cr1 P2 86.99(7) . . ?
C16 Cr1 P2 96.20(6) . . ?
P1 Cr1 P2 88.75(2) . . ?
N1 P1 C2 92.17(9) . . ?
N1 P1 Cr1 128.33(6) . . ?
C2 P1 Cr1 139.48(7) . . ?
N3 Si1 N1 103.53(8) . . ?
N3 Si1 C12 109.70(9) . . ?
N1 Si1 C12 109.93(9) . . ?
N3 Si1 C11 108.92(9) . . ?
N1 Si1 C11 108.87(10) . . ?
C12 Si1 C11 115.23(11) . . ?
N2 N1 P1 113.78(12) . . ?
N2 N1 Si1 111.78(12) . . ?
P1 N1 Si1 134.34(9) . . ?
C1 C2 C5 125.35(16) . . ?
C1 C2 P1 107.57(14) . . ?
C5 C2 P1 127.08(15) . . ?
N3 P2 C7 91.97(9) . . ?
N3 P2 Cr1 125.90(6) . . ?
C7 P2 Cr1 140.03(7) . . ?
C1 N2 N1 109.55(15) . . ?
N2 C1 C2 116.93(16) . . ?
N2 C1 C3 118.22(17) . . ?
C2 C1 C3 124.83(18) . . ?
N4 N3 P2 113.73(12) . . ?
N4 N3 Si1 109.82(12) . . ?
P2 N3 Si1 136.38(10) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 N4 N3 109.44(16) . . ?
C1 C3 C4 112.19(17) . . ?
C1 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
C1 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C7 C10 124.07(17) . . ?
C6 C7 P2 107.68(13) . . ?
C10 C7 P2 128.25(16) . . ?
N4 C6 C7 117.17(17) . . ?
N4 C6 C8 119.46(18) . . ?
C7 C6 C8 123.37(17) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C8 C9 114.47(17) . . ?
C6 C8 H8A 108.6 . . ?
C9 C8 H8A 108.6 . . ?
C6 C8 H8B 108.6 . . ?
C9 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C13 Cr1 175.95(19) . . ?
O2 C14 Cr1 177.1(2) . . ?
O4 C16 Cr1 176.99(18) . . ?
O3 C15 Cr1 177.5(2) . . ?

_refine_diff_density_max         0.317
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.061

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me151207P1_K_1
_database_code_depnum_ccdc_archive 'CCDC 1920914'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H11 N2 P'
_chemical_formula_sum            'C6 H11 N2 P'
_chemical_formula_weight         142.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4900(3)
_cell_length_b                   9.8539(3)
_cell_length_c                   17.6490(4)
_cell_angle_alpha                90
_cell_angle_beta                 121.110(9)
_cell_angle_gamma                90
_cell_volume                     3199.8(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    10722
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_F_000             1216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.582
_exptl_crystal_size_mid          0.361
_exptl_crystal_size_min          0.166
_exptl_absorpt_coefficient_mu    0.263
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.250
0 -1 0 0.291
1 0 -1 0.083
-1 0 1 0.071
1 0 0 0.146
-1 0 0 0.097
1 -1 0 0.263


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            10722
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.214
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3632
_reflns_number_gt                2772
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²+7.1250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3632
_refine_ls_number_parameters     173
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1493
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P2 P 0.09004(4) 0.04565(7) 0.36750(4) 0.02991(19) Uani 1 1 d . . . . .
P1 P -0.06063(4) -0.52533(8) 0.34226(6) 0.0458(2) Uani 1 1 d . . . . .
N4 N 0.10210(11) -0.1262(2) 0.26576(14) 0.0265(4) Uani 1 1 d . . . . .
C7 C 0.11752(13) -0.0055(2) 0.24585(16) 0.0233(5) Uani 1 1 d . . . . .
N1 N -0.02938(12) -0.3763(2) 0.33327(15) 0.0338(5) Uani 1 1 d . . . . .
H1 H -0.0540 -0.3118 0.3066 0.041 Uiso 1 1 d R U . . .
N2 N 0.04333(11) -0.3599(2) 0.37708(14) 0.0297(5) Uani 1 1 d . . . . .
N3 N 0.08715(11) -0.1101(2) 0.33122(14) 0.0282(5) Uani 1 1 d . . . . .
H3 H 0.0757 -0.1855 0.3473 0.034 Uiso 1 1 d R U . . .
C1 C 0.07520(13) -0.4744(2) 0.41979(16) 0.0260(5) Uani 1 1 d . . . . .
C8 C 0.11376(13) 0.1021(2) 0.29490(16) 0.0279(5) Uani 1 1 d . . . . .
H8 H 0.1230 0.1924 0.2887 0.034 Uiso 1 1 d R U . . .
C4 C 0.18751(16) -0.3642(3) 0.53971(19) 0.0392(6) Uani 1 1 d . . . . .
H4A H 0.1747 -0.2794 0.5084 0.047 Uiso 1 1 d R U . . .
H4B H 0.2394 -0.3715 0.5754 0.047 Uiso 1 1 d R U . . .
H4C H 0.1672 -0.3680 0.5770 0.047 Uiso 1 1 d R U . . .
C2 C 0.02670(15) -0.5774(3) 0.40857(19) 0.0376(6) Uani 1 1 d . . . . .
H2 H 0.0403 -0.6632 0.4339 0.045 Uiso 1 1 d R U . . .
C3 C 0.15760(14) -0.4815(3) 0.47382(17) 0.0283(5) Uani 1 1 d . . . . .
C9 C 0.13710(15) 0.0078(3) 0.17496(17) 0.0324(6) Uani 1 1 d D . . . .
C5 C 0.18760(17) -0.4713(4) 0.4119(2) 0.0451(7) Uani 1 1 d . . . . .
H5A H 0.1694 -0.5453 0.3706 0.054 Uiso 1 1 d R U . . .
H5B H 0.2397 -0.4754 0.4464 0.054 Uiso 1 1 d R U . . .
H5C H 0.1727 -0.3869 0.3803 0.054 Uiso 1 1 d R U . . .
C6 C 0.18246(15) -0.6150(3) 0.5249(2) 0.0419(7) Uani 1 1 d . . . . .
H6A H 0.1631 -0.6220 0.5631 0.050 Uiso 1 1 d R U . . .
H6B H 0.2346 -0.6170 0.5598 0.050 Uiso 1 1 d R U . . .
H6C H 0.1653 -0.6897 0.4842 0.050 Uiso 1 1 d R U . . .
C10 C 0.08229(18) 0.1042(3) 0.1015(2) 0.0400(8) Uani 0.900(5) 1 d D . P A 1
H10A H 0.0833 0.1910 0.1268 0.060 Uiso 0.900(5) 1 calc R U P A 1
H10B H 0.0343 0.0664 0.0749 0.060 Uiso 0.900(5) 1 calc R U P A 1
H10C H 0.0953 0.1149 0.0573 0.060 Uiso 0.900(5) 1 calc R U P A 1
C11 C 0.21182(19) 0.0727(6) 0.2154(3) 0.0721(16) Uani 0.900(5) 1 d D . P A 1
H11A H 0.2121 0.1576 0.2423 0.108 Uiso 0.900(5) 1 calc R U P A 1
H11B H 0.2230 0.0883 0.1700 0.108 Uiso 0.900(5) 1 calc R U P A 1
H11C H 0.2476 0.0133 0.2595 0.108 Uiso 0.900(5) 1 calc R U P A 1
C12 C 0.1334(3) -0.1267(3) 0.1316(3) 0.0767(17) Uani 0.900(5) 1 d D . P A 1
H12A H 0.1461 -0.1138 0.0873 0.115 Uiso 0.900(5) 1 calc R U P A 1
H12B H 0.0850 -0.1624 0.1044 0.115 Uiso 0.900(5) 1 calc R U P A 1
H12C H 0.1668 -0.1894 0.1754 0.115 Uiso 0.900(5) 1 calc R U P A 1
C10A C 0.0713(9) 0.010(3) 0.0848(10) 0.0400(8) Uani 0.100(5) 1 d D . P A 2
H10D H 0.0419 -0.0685 0.0772 0.060 Uiso 0.100(5) 1 calc R U P A 2
H10E H 0.0856 0.0080 0.0415 0.060 Uiso 0.100(5) 1 calc R U P A 2
H10F H 0.0438 0.0906 0.0774 0.060 Uiso 0.100(5) 1 calc R U P A 2
C11A C 0.1844(14) 0.132(2) 0.196(2) 0.0721(16) Uani 0.100(5) 1 d D . P A 2
H11D H 0.2283 0.1206 0.2520 0.108 Uiso 0.100(5) 1 calc R U P A 2
H11E H 0.1587 0.2104 0.1975 0.108 Uiso 0.100(5) 1 calc R U P A 2
H11F H 0.1963 0.1440 0.1506 0.108 Uiso 0.100(5) 1 calc R U P A 2
C12A C 0.1826(16) -0.121(2) 0.192(2) 0.0767(17) Uani 0.100(5) 1 d D . P A 2
H12D H 0.2228 -0.1204 0.2520 0.115 Uiso 0.100(5) 1 calc R U P A 2
H12E H 0.2007 -0.1229 0.1523 0.115 Uiso 0.100(5) 1 calc R U P A 2
H12F H 0.1530 -0.1992 0.1824 0.115 Uiso 0.100(5) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P2 N3 1.652(2) . ?
P2 C8 1.699(2) . ?
P1 N1 1.657(2) . ?
P1 C2 1.698(3) . ?
N4 C7 1.330(3) . ?
N4 N3 1.359(3) . ?
C7 C8 1.398(3) . ?
C7 C9 1.518(3) . ?
N1 N2 1.348(3) . ?
N1 H1 0.8051 . ?
N2 C1 1.332(3) . ?
N3 H3 0.8743 . ?
C1 C2 1.394(3) . ?
C1 C3 1.518(3) . ?
C8 H8 0.9300 . ?
C4 C3 1.527(4) . ?
C4 H4A 0.9599 . ?
C4 H4B 0.9599 . ?
C4 H4C 0.9602 . ?
C2 H2 0.9300 . ?
C3 C6 1.527(4) . ?
C3 C5 1.532(4) . ?
C9 C10A 1.486(9) . ?
C9 C11A 1.511(9) . ?
C9 C12 1.513(4) . ?
C9 C11 1.521(4) . ?
C9 C12A 1.531(9) . ?
C9 C10 1.546(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9602 . ?
C6 H6B 0.9598 . ?
C6 H6C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10A H10D 0.9600 . ?
C10A H10E 0.9600 . ?
C10A H10F 0.9600 . ?
C11A H11D 0.9600 . ?
C11A H11E 0.9600 . ?
C11A H11F 0.9600 . ?
C12A H12D 0.9600 . ?
C12A H12E 0.9600 . ?
C12A H12F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 P2 C8 88.73(11) . . ?
N1 P1 C2 88.59(12) . . ?
C7 N4 N3 108.73(19) . . ?
N4 C7 C8 114.4(2) . . ?
N4 C7 C9 120.6(2) . . ?
C8 C7 C9 125.0(2) . . ?
N2 N1 P1 117.27(17) . . ?
N2 N1 H1 117.3 . . ?
P1 N1 H1 125.4 . . ?
C1 N2 N1 109.14(19) . . ?
N4 N3 P2 117.38(15) . . ?
N4 N3 H3 114.0 . . ?
P2 N3 H3 128.6 . . ?
N2 C1 C2 114.1(2) . . ?
N2 C1 C3 119.1(2) . . ?
C2 C1 C3 126.8(2) . . ?
C7 C8 P2 110.76(18) . . ?
C7 C8 H8 124.6 . . ?
P2 C8 H8 124.6 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.3 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C2 P1 110.92(19) . . ?
C1 C2 H2 124.6 . . ?
P1 C2 H2 124.5 . . ?
C1 C3 C4 109.8(2) . . ?
C1 C3 C6 110.5(2) . . ?
C4 C3 C6 108.8(2) . . ?
C1 C3 C5 109.5(2) . . ?
C4 C3 C5 109.1(2) . . ?
C6 C3 C5 109.3(2) . . ?
C10A C9 C11A 113.5(9) . . ?
C10A C9 C7 111.6(11) . . ?
C11A C9 C7 108.0(14) . . ?
C12 C9 C7 112.2(2) . . ?
C12 C9 C11 111.9(3) . . ?
C7 C9 C11 108.9(2) . . ?
C10A C9 C12A 112.2(8) . . ?
C11A C9 C12A 109.9(8) . . ?
C7 C9 C12A 100.8(13) . . ?
C12 C9 C10 107.2(3) . . ?
C7 C9 C10 109.2(2) . . ?
C11 C9 C10 107.3(3) . . ?
C3 C5 H5A 109.7 . . ?
C3 C5 H5B 109.2 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.3 . . ?
C3 C6 H6B 109.4 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.7 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C10A H10D 109.5 . . ?
C9 C10A H10E 109.5 . . ?
H10D C10A H10E 109.5 . . ?
C9 C10A H10F 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
C9 C11A H11D 109.5 . . ?
C9 C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C9 C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C9 C12A H12D 109.5 . . ?
C9 C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C9 C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 N4 0.81 2.16 2.957(3) 169.0 2
N3 H3 N2 0.87 2.02 2.896(3) 176.4 .
N1 H1 N4 0.81 2.16 2.957(3) 169.0 2
N3 H3 N2 0.87 2.02 2.896(3) 176.4 .

_refine_diff_density_max         0.809
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me171005Ni1_6
_database_code_depnum_ccdc_archive 'CCDC 1920915'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H52 N8 Ni P4 Si2'
_chemical_formula_sum            'C28 H52 N8 Ni P4 Si2'
_chemical_formula_weight         739.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.100(3)
_cell_length_b                   18.049(4)
_cell_length_c                   15.439(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.088(6)
_cell_angle_gamma                90
_cell_volume                     3976.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    94929
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.554
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.227
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5938
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.796
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            94929
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9133
_reflns_number_gt                6827
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0321P)²+4.0520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9133
_refine_ls_number_parameters     417
_refine_ls_number_restraints     453
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0826
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.53440(2) 0.62392(2) 0.75737(2) 0.02086(8) Uani 1 1 d . U . . .
P1 P 0.65798(5) 0.56125(4) 0.77648(4) 0.02328(14) Uani 1 1 d . U . . .
Si1 Si 0.67069(5) 0.57185(4) 0.57599(4) 0.02182(15) Uani 1 1 d . U . . .
N1 N 0.78113(15) 0.50025(12) 0.71628(14) 0.0282(5) Uani 1 1 d . U . . .
C1 C 0.74116(18) 0.50743(14) 0.84874(16) 0.0274(6) Uani 1 1 d . U . . .
H1 H 0.7470 0.4976 0.9108 0.033 Uiso 1 1 calc R U . . .
P2 P 0.51196(5) 0.66433(3) 0.62252(4) 0.02191(14) Uani 1 1 d . U . . .
Si2 Si 0.39672(5) 0.63560(4) 0.94664(4) 0.02168(15) Uani 1 1 d . U . . .
N2 N 0.70341(14) 0.54643(11) 0.69254(13) 0.0243(4) Uani 1 1 d . U . . .
C2 C 0.80050(18) 0.47937(14) 0.80258(16) 0.0262(5) Uani 1 1 d . U . . .
P3 P 0.54620(5) 0.70194(4) 0.86317(4) 0.02360(14) Uani 1 1 d . U . . .
N3 N 0.57567(14) 0.63386(11) 0.55883(13) 0.0226(4) Uani 1 1 d . U . . .
C3 C 0.8868(2) 0.43125(16) 0.84454(18) 0.0363(7) Uani 1 1 d . U . . .
N4 N 0.54587(15) 0.65902(12) 0.46913(13) 0.0265(5) Uani 1 1 d . U . . .
P4 P 0.42592(4) 0.55645(3) 0.77353(4) 0.02080(13) Uani 1 1 d . U . . .
C4 C 0.8783(3) 0.3881(2) 0.9263(2) 0.0576(10) Uani 1 1 d . U . . .
H4A H 0.8215 0.3575 0.9067 0.086 Uiso 1 1 calc R U . . .
H4B H 0.8745 0.4228 0.9738 0.086 Uiso 1 1 calc R U . . .
H4C H 0.9333 0.3562 0.9511 0.086 Uiso 1 1 calc R U . . .
N5 N 0.50086(16) 0.75368(11) 0.99878(15) 0.0290(5) Uani 1 1 d . U . . .
C5 C 0.9719(2) 0.4833(2) 0.8751(2) 0.0579(9) Uani 1 1 d . U . . .
H5A H 0.9799 0.5074 0.8213 0.087 Uiso 1 1 calc R U . . .
H5B H 1.0282 0.4546 0.9071 0.087 Uiso 1 1 calc R U . . .
H5C H 0.9618 0.5211 0.9165 0.087 Uiso 1 1 calc R U . . .
N6 N 0.48039(15) 0.69877(11) 0.93200(13) 0.0246(4) Uani 1 1 d . U . . .
C6 C 0.9002(2) 0.37689(18) 0.7739(2) 0.0490(8) Uani 1 1 d . U . . .
H6A H 0.8465 0.3431 0.7541 0.074 Uiso 1 1 calc R U . . .
H6B H 0.9577 0.3483 0.8014 0.074 Uiso 1 1 calc R U . . .
H6C H 0.9049 0.4044 0.7209 0.074 Uiso 1 1 calc R U . . .
N7 N 0.31723(15) 0.51556(11) 0.86372(14) 0.0264(5) Uani 1 1 d . U . . .
C7 C 0.7688(2) 0.62026(17) 0.5547(2) 0.0424(7) Uani 1 1 d . U . . .
H7A H 0.7503 0.6352 0.4902 0.064 Uiso 1 1 calc R U . . .
H7B H 0.8230 0.5871 0.5687 0.064 Uiso 1 1 calc R U . . .
H7C H 0.7854 0.6643 0.5938 0.064 Uiso 1 1 calc R U . . .
C8 C 0.6300(2) 0.48817(15) 0.50581(18) 0.0358(6) Uani 1 1 d . U . . .
H8A H 0.5972 0.5026 0.4422 0.054 Uiso 1 1 calc R U . . .
H8B H 0.5873 0.4603 0.5296 0.054 Uiso 1 1 calc R U . . .
H8C H 0.6840 0.4571 0.5083 0.054 Uiso 1 1 calc R U . . .
N8 N 0.38009(14) 0.56993(11) 0.85773(13) 0.0225(4) Uani 1 1 d . U . . .
C9 C 0.44234(18) 0.71309(13) 0.53238(16) 0.0250(5) Uani 1 1 d . U . . .
H9 H 0.3909 0.7430 0.5332 0.030 Uiso 1 1 calc R U . . .
C10 C 0.47231(18) 0.70261(13) 0.45576(16) 0.0246(5) Uani 1 1 d . U . . .
C11 C 0.4267(2) 0.73445(16) 0.35968(17) 0.0338(6) Uani 1 1 d D U . . .
C15 C 0.60498(18) 0.77584(13) 0.92023(17) 0.0258(5) Uani 1 1 d . U . . .
H15 H 0.6546 0.8005 0.9069 0.031 Uiso 1 1 calc R U . . .
C16 C 0.56948(18) 0.79567(13) 0.99084(17) 0.0255(5) Uani 1 1 d . U . . .
C17 C 0.6046(2) 0.86119(14) 1.05459(19) 0.0334(6) Uani 1 1 d . U . . .
C18 C 0.5526(3) 0.8674(2) 1.1226(3) 0.0841(14) Uani 1 1 d . U . . .
H18A H 0.4875 0.8818 1.0906 0.126 Uiso 1 1 calc R U . . .
H18B H 0.5827 0.9050 1.1687 0.126 Uiso 1 1 calc R U . . .
H18C H 0.5538 0.8195 1.1529 0.126 Uiso 1 1 calc R U . . .
C19 C 0.7094(3) 0.8521(2) 1.1054(2) 0.0615(10) Uani 1 1 d . U . . .
H19A H 0.7425 0.8458 1.0609 0.092 Uiso 1 1 calc R U . . .
H19B H 0.7197 0.8084 1.1452 0.092 Uiso 1 1 calc R U . . .
H19C H 0.7331 0.8963 1.1427 0.092 Uiso 1 1 calc R U . . .
C20 C 0.5931(3) 0.93121(17) 0.9961(2) 0.0610(10) Uani 1 1 d . U . . .
H20A H 0.6261 0.9249 0.9515 0.091 Uiso 1 1 calc R U . . .
H20B H 0.6195 0.9737 1.0357 0.091 Uiso 1 1 calc R U . . .
H20C H 0.5264 0.9400 0.9636 0.091 Uiso 1 1 calc R U . . .
C21 C 0.4472(2) 0.58864(17) 1.05748(18) 0.0393(7) Uani 1 1 d . U . . .
H21A H 0.4051 0.5488 1.0628 0.059 Uiso 1 1 calc R U . . .
H21B H 0.4550 0.6244 1.1072 0.059 Uiso 1 1 calc R U . . .
H21C H 0.5083 0.5677 1.0616 0.059 Uiso 1 1 calc R U . . .
C22 C 0.2850(2) 0.68279(16) 0.9320(2) 0.0417(7) Uani 1 1 d . U . . .
H22A H 0.2614 0.7045 0.8705 0.063 Uiso 1 1 calc R U . . .
H22B H 0.2946 0.7221 0.9780 0.063 Uiso 1 1 calc R U . . .
H22C H 0.2393 0.6470 0.9397 0.063 Uiso 1 1 calc R U . . .
C23 C 0.36333(17) 0.47777(13) 0.74142(16) 0.0246(5) Uani 1 1 d . U . . .
H23 H 0.3645 0.4466 0.6922 0.030 Uiso 1 1 calc R U . . .
C24 C 0.30894(17) 0.46538(13) 0.79907(16) 0.0241(5) Uani 1 1 d . U . . .
C25 C 0.2424(2) 0.40040(14) 0.79193(18) 0.0326(6) Uani 1 1 d . U . . .
C26 C 0.2339(3) 0.3817(2) 0.8837(2) 0.0752(13) Uani 1 1 d . U . . .
H26A H 0.2101 0.4248 0.9077 0.113 Uiso 1 1 calc R U . . .
H26B H 0.2956 0.3680 0.9263 0.113 Uiso 1 1 calc R U . . .
H26C H 0.1906 0.3401 0.8770 0.113 Uiso 1 1 calc R U . . .
C27 C 0.1486(3) 0.4196(2) 0.7236(3) 0.0935(16) Uani 1 1 d . U . . .
H27A H 0.1564 0.4326 0.6648 0.140 Uiso 1 1 calc R U . . .
H27B H 0.1217 0.4618 0.7462 0.140 Uiso 1 1 calc R U . . .
H27C H 0.1065 0.3769 0.7151 0.140 Uiso 1 1 calc R U . . .
C28 C 0.2790(4) 0.3323(2) 0.7567(4) 0.0925(16) Uani 1 1 d . U . . .
H28A H 0.2346 0.2914 0.7497 0.139 Uiso 1 1 calc R U . . .
H28B H 0.3399 0.3182 0.8005 0.139 Uiso 1 1 calc R U . . .
H28C H 0.2862 0.3435 0.6973 0.139 Uiso 1 1 calc R U . . .
C12 C 0.5023(3) 0.7756(3) 0.3312(3) 0.0610(12) Uani 0.838(3) 1 d D U P A 1
H12A H 0.4743 0.7957 0.2692 0.091 Uiso 0.838(3) 1 calc R U P A 1
H12B H 0.5526 0.7411 0.3319 0.091 Uiso 0.838(3) 1 calc R U P A 1
H12C H 0.5280 0.8162 0.3742 0.091 Uiso 0.838(3) 1 calc R U P A 1
C13 C 0.3881(4) 0.6707(3) 0.2945(3) 0.0699(13) Uani 0.838(3) 1 d D U P A 1
H13A H 0.3620 0.6897 0.2318 0.105 Uiso 0.838(3) 1 calc R U P A 1
H13B H 0.3387 0.6456 0.3117 0.105 Uiso 0.838(3) 1 calc R U P A 1
H13C H 0.4385 0.6355 0.2979 0.105 Uiso 0.838(3) 1 calc R U P A 1
C14 C 0.3502(3) 0.7899(3) 0.3584(3) 0.0624(12) Uani 0.838(3) 1 d D U P A 1
H14A H 0.3249 0.8118 0.2972 0.094 Uiso 0.838(3) 1 calc R U P A 1
H14B H 0.3766 0.8290 0.4035 0.094 Uiso 0.838(3) 1 calc R U P A 1
H14C H 0.2999 0.7644 0.3737 0.094 Uiso 0.838(3) 1 calc R U P A 1
C12A C 0.4322(15) 0.8203(7) 0.3599(13) 0.0610(12) Uani 0.162(3) 1 d D U P A 2
H12D H 0.4979 0.8357 0.3761 0.091 Uiso 0.162(3) 1 calc R U P A 2
H12F H 0.4054 0.8402 0.4050 0.091 Uiso 0.162(3) 1 calc R U P A 2
H12E H 0.3969 0.8392 0.2989 0.091 Uiso 0.162(3) 1 calc R U P A 2
C13A C 0.4752(14) 0.7058(12) 0.2907(12) 0.0699(13) Uani 0.162(3) 1 d D U P A 2
H13E H 0.4717 0.6516 0.2877 0.105 Uiso 0.162(3) 1 calc R U P A 2
H13F H 0.5410 0.7213 0.3115 0.105 Uiso 0.162(3) 1 calc R U P A 2
H13D H 0.4433 0.7265 0.2298 0.105 Uiso 0.162(3) 1 calc R U P A 2
C14A C 0.3224(10) 0.7105(11) 0.3240(13) 0.0624(12) Uani 0.162(3) 1 d D U P A 2
H14E H 0.2948 0.7248 0.2595 0.094 Uiso 0.162(3) 1 calc R U P A 2
H14F H 0.2884 0.7349 0.3602 0.094 Uiso 0.162(3) 1 calc R U P A 2
H14D H 0.3182 0.6566 0.3297 0.094 Uiso 0.162(3) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P1 2.1187(8) . ?
Ni1 P3 2.1195(7) . ?
Ni1 P4 2.1204(8) . ?
Ni1 P2 2.1260(8) . ?
P1 N2 1.674(2) . ?
P1 C1 1.688(3) . ?
Si1 N2 1.764(2) . ?
Si1 N3 1.770(2) . ?
Si1 C7 1.840(3) . ?
Si1 C8 1.843(3) . ?
N1 C2 1.322(3) . ?
N1 N2 1.387(3) . ?
C1 C2 1.409(3) . ?
C1 H1 0.9500 . ?
P2 N3 1.677(2) . ?
P2 C9 1.691(2) . ?
Si2 N8 1.768(2) . ?
Si2 N6 1.770(2) . ?
Si2 C22 1.837(3) . ?
Si2 C21 1.837(3) . ?
C2 C3 1.524(4) . ?
P3 N6 1.677(2) . ?
P3 C15 1.683(3) . ?
N3 N4 1.385(3) . ?
C3 C4 1.525(4) . ?
C3 C6 1.529(4) . ?
C3 C5 1.536(4) . ?
N4 C10 1.321(3) . ?
P4 N8 1.678(2) . ?
P4 C23 1.688(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N5 C16 1.321(3) . ?
N5 N6 1.390(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N7 C24 1.323(3) . ?
N7 N8 1.389(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.411(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.529(3) . ?
C11 C13 1.514(5) . ?
C11 C14 1.524(5) . ?
C11 C12 1.542(5) . ?
C11 C14A 1.550(13) . ?
C11 C12A 1.552(13) . ?
C11 C13A 1.564(13) . ?
C15 C16 1.409(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.519(3) . ?
C17 C18 1.507(4) . ?
C17 C19 1.528(4) . ?
C17 C20 1.530(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.412(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.525(3) . ?
C25 C26 1.502(4) . ?
C25 C27 1.505(5) . ?
C25 C28 1.519(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12F 0.9800 . ?
C12A H12E 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
C13A H13D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C14A H14D 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Ni1 P3 113.52(3) . . ?
P1 Ni1 P4 110.86(3) . . ?
P3 Ni1 P4 99.46(3) . . ?
P1 Ni1 P2 99.82(3) . . ?
P3 Ni1 P2 118.24(3) . . ?
P4 Ni1 P2 115.49(3) . . ?
N2 P1 C1 90.86(11) . . ?
N2 P1 Ni1 122.87(8) . . ?
C1 P1 Ni1 146.14(9) . . ?
N2 Si1 N3 105.08(9) . . ?
N2 Si1 C7 109.43(13) . . ?
N3 Si1 C7 109.49(12) . . ?
N2 Si1 C8 108.35(12) . . ?
N3 Si1 C8 109.41(12) . . ?
C7 Si1 C8 114.64(14) . . ?
C2 N1 N2 109.1(2) . . ?
C2 C1 P1 109.34(18) . . ?
C2 C1 H1 125.3 . . ?
P1 C1 H1 125.3 . . ?
N3 P2 C9 90.54(11) . . ?
N3 P2 Ni1 121.55(7) . . ?
C9 P2 Ni1 147.31(9) . . ?
N8 Si2 N6 104.99(9) . . ?
N8 Si2 C22 108.90(13) . . ?
N6 Si2 C22 110.53(12) . . ?
N8 Si2 C21 108.92(12) . . ?
N6 Si2 C21 108.68(12) . . ?
C22 Si2 C21 114.39(14) . . ?
N1 N2 P1 114.64(15) . . ?
N1 N2 Si1 110.87(15) . . ?
P1 N2 Si1 134.36(13) . . ?
N1 C2 C1 116.1(2) . . ?
N1 C2 C3 117.9(2) . . ?
C1 C2 C3 125.9(2) . . ?
N6 P3 C15 90.89(11) . . ?
N6 P3 Ni1 123.23(7) . . ?
C15 P3 Ni1 145.81(9) . . ?
N4 N3 P2 114.68(16) . . ?
N4 N3 Si1 109.84(15) . . ?
P2 N3 Si1 135.38(12) . . ?
C2 C3 C4 110.5(2) . . ?
C2 C3 C6 110.9(2) . . ?
C4 C3 C6 109.3(3) . . ?
C2 C3 C5 107.2(2) . . ?
C4 C3 C5 110.3(3) . . ?
C6 C3 C5 108.6(3) . . ?
C10 N4 N3 109.45(19) . . ?
N8 P4 C23 90.94(11) . . ?
N8 P4 Ni1 122.55(7) . . ?
C23 P4 Ni1 145.95(9) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C16 N5 N6 109.3(2) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 N6 P3 114.31(16) . . ?
N5 N6 Si2 111.06(15) . . ?
P3 N6 Si2 134.31(12) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C24 N7 N8 109.4(2) . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 N8 P4 114.39(15) . . ?
N7 N8 Si2 110.40(15) . . ?
P4 N8 Si2 135.13(12) . . ?
C10 C9 P2 109.68(19) . . ?
C10 C9 H9 125.2 . . ?
P2 C9 H9 125.2 . . ?
N4 C10 C9 115.6(2) . . ?
N4 C10 C11 117.7(2) . . ?
C9 C10 C11 126.7(2) . . ?
C13 C11 C14 111.4(3) . . ?
C13 C11 C10 108.2(2) . . ?
C14 C11 C10 111.0(2) . . ?
C13 C11 C12 109.7(3) . . ?
C14 C11 C12 108.0(3) . . ?
C10 C11 C12 108.5(2) . . ?
C10 C11 C14A 108.8(7) . . ?
C10 C11 C12A 111.5(7) . . ?
C14A C11 C12A 109.1(9) . . ?
C10 C11 C13A 111.9(8) . . ?
C14A C11 C13A 108.2(9) . . ?
C12A C11 C13A 107.2(10) . . ?
C16 C15 P3 109.72(18) . . ?
C16 C15 H15 125.1 . . ?
P3 C15 H15 125.1 . . ?
N5 C16 C15 115.7(2) . . ?
N5 C16 C17 120.3(2) . . ?
C15 C16 C17 124.0(2) . . ?
C18 C17 C16 111.0(2) . . ?
C18 C17 C19 109.8(3) . . ?
C16 C17 C19 109.4(2) . . ?
C18 C17 C20 111.5(3) . . ?
C16 C17 C20 108.2(2) . . ?
C19 C17 C20 106.8(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P4 109.47(18) . . ?
C24 C23 H23 125.3 . . ?
P4 C23 H23 125.3 . . ?
N7 C24 C23 115.9(2) . . ?
N7 C24 C25 118.6(2) . . ?
C23 C24 C25 125.5(2) . . ?
C26 C25 C27 111.2(3) . . ?
C26 C25 C28 108.0(3) . . ?
C27 C25 C28 107.7(3) . . ?
C26 C25 C24 111.2(2) . . ?
C27 C25 C24 108.7(2) . . ?
C28 C25 C24 109.9(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C12A H12D 109.5 . . ?
C11 C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
C11 C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12F C12A H12E 109.5 . . ?
C11 C13A H13E 109.5 . . ?
C11 C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C11 C13A H13D 109.5 . . ?
H13E C13A H13D 109.5 . . ?
H13F C13A H13D 109.5 . . ?
C11 C14A H14E 109.5 . . ?
C11 C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C11 C14A H14D 109.5 . . ?
H14E C14A H14D 109.5 . . ?
H14F C14A H14D 109.5 . . ?

_refine_diff_density_max         0.542
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.069

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me180409Br_12
_database_code_depnum_ccdc_archive 'CCDC 1920920'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H22 Br2 Co N4 P2 Si'
_chemical_formula_sum            'C12 H22 Br2 Co N4 P2 Si'
_chemical_formula_weight         531.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.9431(12)
_cell_length_b                   9.3567(10)
_cell_length_c                   21.837(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.989(4)
_cell_angle_gamma                90
_cell_volume                     2011.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    46141
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    5.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4426
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.594
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            46141
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_av_R_equivalents  0.1731
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.150
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4622
_reflns_number_gt                3486
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0541P)²+27.6262P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4622
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0842
_refine_ls_wR_factor_ref         0.1885
_refine_ls_wR_factor_gt          0.1765
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.28474(10) 0.33033(11) 0.56376(5) 0.0296(3) Uani 1 1 d . . . . .
Co1 Co 0.47859(11) 0.28063(12) 0.63641(5) 0.0161(3) Uani 1 1 d . . . . .
P1 P 0.5863(2) 0.6189(2) 0.78399(11) 0.0223(5) Uani 1 1 d . . . . .
Si1 Si 0.6527(2) 0.5931(2) 0.65200(11) 0.0167(5) Uani 1 1 d . . . . .
N1 N 0.4865(7) 0.4218(7) 0.7085(3) 0.0178(15) Uani 1 1 d . . . . .
C1 C 0.4168(8) 0.4150(9) 0.7571(4) 0.0171(17) Uani 1 1 d . . . . .
P2 P 0.8763(3) 0.4586(3) 0.58861(12) 0.0274(6) Uani 1 1 d . . . . .
Br2 Br 0.49964(10) 0.04249(10) 0.67583(5) 0.0263(2) Uani 1 1 d . . . . .
N2 N 0.5812(7) 0.5282(8) 0.7169(3) 0.0181(15) Uani 1 1 d . . . . .
C2 C 0.4571(8) 0.5157(10) 0.8040(4) 0.0193(18) Uani 1 1 d . . . . .
N3 N 0.6512(7) 0.3301(7) 0.5991(3) 0.0183(15) Uani 1 1 d . . . . .
C3 C 0.7099(8) 0.2547(9) 0.5581(4) 0.0154(17) Uani 1 1 d . . . . .
N4 N 0.7312(7) 0.4435(7) 0.6207(3) 0.0193(15) Uani 1 1 d . . . . .
C4 C 0.8357(9) 0.3105(10) 0.5455(4) 0.0222(19) Uani 1 1 d . . . . .
C5 C 0.3011(10) 0.3104(10) 0.7572(4) 0.026(2) Uani 1 1 d . . . . .
H5A H 0.2839 0.2641 0.7161 0.031 Uiso 1 1 calc R U . . .
H5B H 0.2183 0.3643 0.7632 0.031 Uiso 1 1 calc R U . . .
C6 C 0.3245(12) 0.1952(12) 0.8060(5) 0.037(3) Uani 1 1 d . . . . .
H6A H 0.2388 0.1456 0.8089 0.055 Uiso 1 1 calc R U . . .
H6B H 0.3583 0.2387 0.8461 0.055 Uiso 1 1 calc R U . . .
H6C H 0.3915 0.1267 0.7948 0.055 Uiso 1 1 calc R U . . .
C7 C 0.3982(10) 0.5307(12) 0.8631(4) 0.031(2) Uani 1 1 d . . . . .
H7A H 0.2989 0.5266 0.8544 0.047 Uiso 1 1 calc R U . . .
H7B H 0.4259 0.6226 0.8824 0.047 Uiso 1 1 calc R U . . .
H7C H 0.4313 0.4528 0.8912 0.047 Uiso 1 1 calc R U . . .
C8 C 0.6451(9) 0.1205(9) 0.5304(4) 0.0185(18) Uani 1 1 d . . . . .
H8A H 0.6414 0.1244 0.4849 0.022 Uiso 1 1 calc R U . . .
H8B H 0.5508 0.1146 0.5399 0.022 Uiso 1 1 calc R U . . .
C9 C 0.7228(10) -0.0132(10) 0.5549(5) 0.028(2) Uani 1 1 d . . . . .
H9A H 0.6812 -0.0976 0.5334 0.042 Uiso 1 1 calc R U . . .
H9B H 0.7194 -0.0223 0.5994 0.042 Uiso 1 1 calc R U . . .
H9C H 0.8176 -0.0054 0.5476 0.042 Uiso 1 1 calc R U . . .
C10 C 0.9152(10) 0.2500(13) 0.4972(5) 0.035(3) Uani 1 1 d . . . . .
H10A H 0.8528 0.2262 0.4598 0.052 Uiso 1 1 calc R U . . .
H10B H 0.9632 0.1635 0.5134 0.052 Uiso 1 1 calc R U . . .
H10C H 0.9812 0.3210 0.4871 0.052 Uiso 1 1 calc R U . . .
C11 C 0.5163(10) 0.6607(10) 0.5945(4) 0.026(2) Uani 1 1 d . . . . .
H11A H 0.5532 0.6853 0.5565 0.039 Uiso 1 1 calc R U . . .
H11B H 0.4763 0.7460 0.6107 0.039 Uiso 1 1 calc R U . . .
H11C H 0.4463 0.5870 0.5855 0.039 Uiso 1 1 calc R U . . .
C12 C 0.7856(10) 0.7220(10) 0.6815(5) 0.028(2) Uani 1 1 d . . . . .
H12A H 0.8405 0.7447 0.6489 0.041 Uiso 1 1 calc R U . . .
H12B H 0.8437 0.6804 0.7170 0.041 Uiso 1 1 calc R U . . .
H12C H 0.7433 0.8095 0.6945 0.041 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Co1 2.3660(15) . ?
Co1 N1 2.048(7) . ?
Co1 N3 2.052(7) . ?
Co1 Br2 2.3874(15) . ?
P1 N2 1.687(8) . ?
P1 C2 1.711(9) . ?
Si1 N2 1.779(7) . ?
Si1 N4 1.784(7) . ?
Si1 C11 1.828(9) . ?
Si1 C12 1.838(10) . ?
N1 C1 1.347(11) . ?
N1 N2 1.366(10) . ?
C1 C2 1.408(12) . ?
C1 C5 1.511(12) . ?
P2 C4 1.692(10) . ?
P2 N4 1.696(8) . ?
C2 C7 1.496(12) . ?
N3 C3 1.337(11) . ?
N3 N4 1.369(10) . ?
C3 C4 1.418(12) . ?
C3 C8 1.500(11) . ?
C4 C10 1.513(12) . ?
C5 C6 1.512(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.527(13) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N3 102.4(3) . . ?
N1 Co1 Br1 109.2(2) . . ?
N3 Co1 Br1 109.8(2) . . ?
N1 Co1 Br2 109.4(2) . . ?
N3 Co1 Br2 108.5(2) . . ?
Br1 Co1 Br2 116.59(6) . . ?
N2 P1 C2 90.3(4) . . ?
N2 Si1 N4 106.4(4) . . ?
N2 Si1 C11 109.0(4) . . ?
N4 Si1 C11 109.3(4) . . ?
N2 Si1 C12 106.9(4) . . ?
N4 Si1 C12 108.5(4) . . ?
C11 Si1 C12 116.3(4) . . ?
C1 N1 N2 110.4(7) . . ?
C1 N1 Co1 127.4(6) . . ?
N2 N1 Co1 121.7(5) . . ?
N1 C1 C2 114.6(8) . . ?
N1 C1 C5 120.4(8) . . ?
C2 C1 C5 124.9(8) . . ?
C4 P2 N4 90.6(4) . . ?
N1 N2 P1 114.8(6) . . ?
N1 N2 Si1 119.1(5) . . ?
P1 N2 Si1 123.6(4) . . ?
C1 C2 C7 125.8(8) . . ?
C1 C2 P1 109.8(7) . . ?
C7 C2 P1 124.4(7) . . ?
C3 N3 N4 110.7(7) . . ?
C3 N3 Co1 127.8(6) . . ?
N4 N3 Co1 121.1(5) . . ?
N3 C3 C4 114.5(8) . . ?
N3 C3 C8 120.7(7) . . ?
C4 C3 C8 124.8(8) . . ?
N3 N4 P2 114.1(6) . . ?
N3 N4 Si1 118.4(6) . . ?
P2 N4 Si1 122.4(4) . . ?
C3 C4 C10 123.9(9) . . ?
C3 C4 P2 110.0(6) . . ?
C10 C4 P2 125.9(7) . . ?
C1 C5 C6 114.9(8) . . ?
C1 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
C1 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 C9 112.1(7) . . ?
C3 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
C3 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         1.853
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.221

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me180226Mo1_11
_database_code_depnum_ccdc_archive 'CCDC 1920917'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 Mo N4 O4 P2 Si'
_chemical_formula_sum            'C16 H22 Mo N4 O4 P2 Si'
_chemical_formula_weight         520.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8860(6)
_cell_length_b                   9.9302(9)
_cell_length_c                   26.122(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.153(3)
_cell_angle_gamma                90
_cell_volume                     2281.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    75562
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.123
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6119
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.820
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            75562
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.338
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5267
_reflns_number_gt                4553
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+0.9676P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5267
_refine_ls_number_parameters     259
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.72820(2) 0.51297(2) 0.68770(2) 0.02134(6) Uani 1 1 d . . . . .
P1 P 0.57132(6) 0.71510(6) 0.67116(2) 0.02345(12) Uani 1 1 d . . . . .
Si1 Si 0.70264(6) 0.85668(6) 0.57648(2) 0.02370(13) Uani 1 1 d . . . . .
O1 O 0.5369(3) 0.4060(2) 0.77166(9) 0.0636(7) Uani 1 1 d . . . . .
N1 N 0.58251(19) 0.82676(19) 0.62367(7) 0.0246(4) Uani 1 1 d . . . . .
C1 C 0.3673(2) 0.8901(2) 0.64972(9) 0.0250(5) Uani 1 1 d . . . . .
P2 P 0.88964(6) 0.60817(6) 0.62949(2) 0.02330(12) Uani 1 1 d . . . . .
O2 O 0.9018(2) 0.23710(18) 0.69022(7) 0.0438(4) Uani 1 1 d . . . . .
N2 N 0.4622(2) 0.91670(19) 0.61668(7) 0.0267(4) Uani 1 1 d . . . . .
C2 C 0.4040(2) 0.7801(2) 0.68363(8) 0.0250(5) Uani 1 1 d . . . . .
O3 O 0.9529(2) 0.6270(2) 0.78418(8) 0.0558(6) Uani 1 1 d . . . . .
N3 N 0.85618(19) 0.74349(19) 0.59160(7) 0.0253(4) Uani 1 1 d . . . . .
C3 C 0.2274(3) 0.9759(2) 0.65016(10) 0.0343(5) Uani 1 1 d . . . . .
H3A H 0.2314 1.0174 0.6848 0.041 Uiso 1 1 calc R U . . .
H3B H 0.1367 0.9168 0.6447 0.041 Uiso 1 1 calc R U . . .
O4 O 0.5142(2) 0.3699(3) 0.59638(9) 0.0694(7) Uani 1 1 d . . . . .
N4 N 0.9710(2) 0.7696(2) 0.56198(7) 0.0292(4) Uani 1 1 d . . . . .
C4 C 0.2081(3) 1.0859(3) 0.60995(14) 0.0528(8) Uani 1 1 d . . . . .
H4A H 0.1994 1.0458 0.5754 0.079 Uiso 1 1 calc R U . . .
H4B H 0.2966 1.1459 0.6152 0.079 Uiso 1 1 calc R U . . .
H4C H 0.1160 1.1376 0.6132 0.079 Uiso 1 1 calc R U . . .
C5 C 0.3083(3) 0.7333(3) 0.72328(9) 0.0369(6) Uani 1 1 d . . . . .
H5A H 0.2055 0.7126 0.7062 0.055 Uiso 1 1 calc R U . . .
H5B H 0.3034 0.8045 0.7490 0.055 Uiso 1 1 calc R U . . .
H5C H 0.3537 0.6523 0.7405 0.055 Uiso 1 1 calc R U . . .
C6 C 1.0797(2) 0.6793(2) 0.57213(9) 0.0265(5) Uani 1 1 d . . . . .
C7 C 1.0592(2) 0.5791(2) 0.60890(9) 0.0267(5) Uani 1 1 d . . . . .
C8 C 1.2144(3) 0.6877(3) 0.54310(10) 0.0358(6) Uani 1 1 d . . . . .
H8A H 1.3068 0.6583 0.5661 0.043 Uiso 1 1 calc R U . . .
H8B H 1.2294 0.7825 0.5333 0.043 Uiso 1 1 calc R U . . .
C9 C 1.1939(4) 0.6014(4) 0.49501(13) 0.0693(10) Uani 1 1 d . U . . .
H9A H 1.1042 0.6319 0.4717 0.104 Uiso 1 1 calc R U . . .
H9B H 1.1801 0.5073 0.5046 0.104 Uiso 1 1 calc R U . . .
H9C H 1.2841 0.6091 0.4775 0.104 Uiso 1 1 calc R U . . .
C10 C 1.1683(3) 0.4681(3) 0.62658(12) 0.0432(7) Uani 1 1 d . . . . .
H10A H 1.1828 0.4111 0.5970 0.065 Uiso 1 1 calc R U . . .
H10B H 1.1275 0.4136 0.6527 0.065 Uiso 1 1 calc R U . . .
H10C H 1.2662 0.5068 0.6416 0.065 Uiso 1 1 calc R U . . .
C11 C 0.7729(3) 1.0302(3) 0.58236(12) 0.0435(7) Uani 1 1 d . . . . .
H11A H 0.8325 1.0493 0.5544 0.065 Uiso 1 1 calc R U . . .
H11B H 0.8371 1.0418 0.6158 0.065 Uiso 1 1 calc R U . . .
H11C H 0.6865 1.0924 0.5800 0.065 Uiso 1 1 calc R U . . .
C12 C 0.6004(3) 0.8117(3) 0.51289(9) 0.0441(7) Uani 1 1 d . . . . .
H12A H 0.6652 0.8298 0.4863 0.066 Uiso 1 1 calc R U . . .
H12B H 0.5073 0.8654 0.5059 0.066 Uiso 1 1 calc R U . . .
H12C H 0.5742 0.7158 0.5125 0.066 Uiso 1 1 calc R U . . .
C13 C 0.6025(3) 0.4440(2) 0.74007(10) 0.0368(6) Uani 1 1 d . . . . .
C14 C 0.8431(3) 0.3390(2) 0.69103(9) 0.0288(5) Uani 1 1 d . . . . .
C15 C 0.8729(3) 0.5899(2) 0.74948(10) 0.0321(5) Uani 1 1 d . . . . .
C16 C 0.5894(3) 0.4241(3) 0.62860(10) 0.0371(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C14 2.003(2) . ?
Mo1 C13 2.005(2) . ?
Mo1 C16 2.035(3) . ?
Mo1 C15 2.062(3) . ?
Mo1 P2 2.4254(6) . ?
Mo1 P1 2.4471(6) . ?
P1 N1 1.6771(19) . ?
P1 C2 1.695(2) . ?
Si1 N1 1.7666(18) . ?
Si1 N3 1.7686(19) . ?
Si1 C11 1.832(3) . ?
Si1 C12 1.832(3) . ?
O1 C13 1.140(3) . ?
N1 N2 1.385(2) . ?
C1 N2 1.316(3) . ?
C1 C2 1.415(3) . ?
C1 C3 1.508(3) . ?
P2 N3 1.6703(19) . ?
P2 C7 1.695(2) . ?
O2 C14 1.140(3) . ?
C2 C5 1.504(3) . ?
O3 C15 1.131(3) . ?
N3 N4 1.390(2) . ?
C3 C4 1.509(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C16 1.134(3) . ?
N4 C6 1.317(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.413(3) . ?
C6 C8 1.507(3) . ?
C7 C10 1.497(3) . ?
C8 C9 1.510(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 Mo1 C13 90.33(10) . . ?
C14 Mo1 C16 84.81(10) . . ?
C13 Mo1 C16 91.91(11) . . ?
C14 Mo1 C15 91.61(9) . . ?
C13 Mo1 C15 86.47(11) . . ?
C16 Mo1 C15 176.06(10) . . ?
C14 Mo1 P2 91.16(6) . . ?
C13 Mo1 P2 175.54(8) . . ?
C16 Mo1 P2 92.41(7) . . ?
C15 Mo1 P2 89.28(7) . . ?
C14 Mo1 P1 171.72(7) . . ?
C13 Mo1 P1 92.41(7) . . ?
C16 Mo1 P1 87.30(8) . . ?
C15 Mo1 P1 96.35(7) . . ?
P2 Mo1 P1 86.695(19) . . ?
N1 P1 C2 92.07(10) . . ?
N1 P1 Mo1 125.51(6) . . ?
C2 P1 Mo1 140.52(8) . . ?
N1 Si1 N3 105.10(8) . . ?
N1 Si1 C11 109.39(11) . . ?
N3 Si1 C11 109.66(11) . . ?
N1 Si1 C12 108.71(11) . . ?
N3 Si1 C12 108.37(12) . . ?
C11 Si1 C12 115.13(14) . . ?
N2 N1 P1 113.48(13) . . ?
N2 N1 Si1 109.32(14) . . ?
P1 N1 Si1 137.08(11) . . ?
N2 C1 C2 116.95(19) . . ?
N2 C1 C3 119.8(2) . . ?
C2 C1 C3 123.2(2) . . ?
N3 P2 C7 92.33(10) . . ?
N3 P2 Mo1 127.85(6) . . ?
C7 P2 Mo1 139.81(9) . . ?
C1 N2 N1 109.78(18) . . ?
C1 C2 C5 124.6(2) . . ?
C1 C2 P1 107.70(15) . . ?
C5 C2 P1 127.74(18) . . ?
N4 N3 P2 113.39(14) . . ?
N4 N3 Si1 111.17(14) . . ?
P2 N3 Si1 135.27(11) . . ?
C1 C3 C4 114.6(2) . . ?
C1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
C1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C6 N4 N3 109.66(18) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 C7 117.06(19) . . ?
N4 C6 C8 118.2(2) . . ?
C7 C6 C8 124.7(2) . . ?
C6 C7 C10 126.0(2) . . ?
C6 C7 P2 107.56(16) . . ?
C10 C7 P2 126.41(18) . . ?
C6 C8 C9 112.1(2) . . ?
C6 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
C6 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 Mo1 176.7(3) . . ?
O2 C14 Mo1 175.5(2) . . ?
O3 C15 Mo1 177.2(2) . . ?
O4 C16 Mo1 177.3(3) . . ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.091

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me180108W1_10
_database_code_depnum_ccdc_archive 'CCDC 1920916'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 N4 O4 P2 Si W'
_chemical_formula_sum            'C16 H22 N4 O4 P2 Si W'
_chemical_formula_weight         608.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8502(12)
_cell_length_b                   9.8645(17)
_cell_length_c                   26.010(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.210(5)
_cell_angle_gamma                90
_cell_volume                     2247.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    56894
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.144
_exptl_absorpt_coefficient_mu    5.364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4073
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.546
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            56894
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_av_R_equivalents  0.1560
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.211
_diffrn_reflns_theta_max         27.627
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5206
_reflns_number_gt                3978
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²+6.6287P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5206
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1009
_refine_ls_wR_factor_gt          0.0913
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.72914(3) 0.48629(2) 0.68812(2) 0.01843(9) Uani 1 1 d . . . . .
C6 C 1.0821(7) 0.3219(6) 0.5724(2) 0.0212(13) Uani 1 1 d . . . . .
N3 N 0.8569(6) 0.2543(5) 0.59116(19) 0.0200(11) Uani 1 1 d . . . . .
Si1 Si 0.70301(19) 0.14160(17) 0.57626(7) 0.0202(4) Uani 1 1 d . . . . .
P2 P 0.89069(18) 0.39155(16) 0.62975(6) 0.0200(3) Uani 1 1 d . . . . .
P1 P 0.57183(18) 0.28431(16) 0.67141(6) 0.0201(3) Uani 1 1 d . . . . .
C7 C 1.0593(7) 0.4198(6) 0.6097(2) 0.0214(13) Uani 1 1 d . . . . .
N4 N 0.9715(6) 0.2297(5) 0.5619(2) 0.0239(12) Uani 1 1 d . . . . .
O4 O 0.9546(6) 0.3706(5) 0.7846(2) 0.0452(14) Uani 1 1 d . . . . .
C10 C 1.1705(8) 0.5329(7) 0.6276(3) 0.0377(18) Uani 1 1 d . . . . .
H10A H 1.1293 0.5882 0.6537 0.057 Uiso 1 1 calc R U . . .
H10B H 1.1854 0.5898 0.5979 0.057 Uiso 1 1 calc R U . . .
H10C H 1.2685 0.4939 0.6429 0.057 Uiso 1 1 calc R U . . .
N2 N 0.4621(6) 0.0816(5) 0.6167(2) 0.0218(11) Uani 1 1 d . . . . .
C9 C 1.1960(10) 0.4012(11) 0.4954(4) 0.064(3) Uani 1 1 d . . . . .
H9A H 1.2857 0.3916 0.4776 0.096 Uiso 1 1 calc R U . . .
H9B H 1.1854 0.4961 0.5055 0.096 Uiso 1 1 calc R U . . .
H9C H 1.1045 0.3731 0.4721 0.096 Uiso 1 1 calc R U . . .
N1 N 0.5839(6) 0.1710(5) 0.6236(2) 0.0207(11) Uani 1 1 d . . . . .
C8 C 1.2150(7) 0.3128(7) 0.5435(3) 0.0309(16) Uani 1 1 d . . . . .
H8A H 1.2283 0.2174 0.5332 0.037 Uiso 1 1 calc R U . . .
H8B H 1.3085 0.3406 0.5666 0.037 Uiso 1 1 calc R U . . .
O3 O 0.5384(7) 0.5929(5) 0.7727(2) 0.0537(17) Uani 1 1 d . . . . .
C1 C 0.3669(7) 0.1089(6) 0.6499(2) 0.0203(13) Uani 1 1 d . . . . .
O2 O 0.9030(6) 0.7639(5) 0.69022(19) 0.0361(12) Uani 1 1 d . . . . .
C2 C 0.4045(7) 0.2211(6) 0.6842(2) 0.0235(14) Uani 1 1 d . . . . .
C4 C 0.2070(8) -0.0873(8) 0.6098(3) 0.043(2) Uani 1 1 d . . . . .
H4A H 0.1133 -0.1380 0.6126 0.064 Uiso 1 1 calc R U . . .
H4B H 0.2947 -0.1489 0.6154 0.064 Uiso 1 1 calc R U . . .
H4C H 0.2002 -0.0468 0.5751 0.064 Uiso 1 1 calc R U . . .
C3 C 0.2269(8) 0.0233(6) 0.6503(3) 0.0277(15) Uani 1 1 d . . . . .
H3A H 0.1361 0.0829 0.6449 0.033 Uiso 1 1 calc R U . . .
H3B H 0.2311 -0.0188 0.6850 0.033 Uiso 1 1 calc R U . . .
O1 O 0.5132(6) 0.6318(7) 0.5966(2) 0.0571(17) Uani 1 1 d . . . . .
C5 C 0.3080(8) 0.2683(8) 0.7240(3) 0.0322(16) Uani 1 1 d . . . . .
H5A H 0.3567 0.3466 0.7427 0.048 Uiso 1 1 calc R U . . .
H5B H 0.2978 0.1947 0.7486 0.048 Uiso 1 1 calc R U . . .
H5C H 0.2066 0.2943 0.7065 0.048 Uiso 1 1 calc R U . . .
C15 C 0.6053(8) 0.5547(6) 0.7412(3) 0.0277(15) Uani 1 1 d . . . . .
C14 C 0.8451(7) 0.6639(7) 0.6910(2) 0.0226(14) Uani 1 1 d . . . . .
C13 C 0.5887(8) 0.5766(8) 0.6289(3) 0.0329(17) Uani 1 1 d . . . . .
C16 C 0.8736(8) 0.4095(6) 0.7494(3) 0.0252(15) Uani 1 1 d . . . . .
C11 C 0.5993(8) 0.1874(8) 0.5126(3) 0.0363(18) Uani 1 1 d . . . . .
H11A H 0.5132 0.1253 0.5036 0.054 Uiso 1 1 calc R U . . .
H11B H 0.6682 0.1809 0.4863 0.054 Uiso 1 1 calc R U . . .
H11C H 0.5613 0.2805 0.5137 0.054 Uiso 1 1 calc R U . . .
C12 C 0.7721(9) -0.0342(7) 0.5824(3) 0.0366(18) Uani 1 1 d . . . . .
H12A H 0.6859 -0.0965 0.5740 0.055 Uiso 1 1 calc R U . . .
H12B H 0.8210 -0.0505 0.6181 0.055 Uiso 1 1 calc R U . . .
H12C H 0.8463 -0.0494 0.5584 0.055 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C15 1.999(7) . ?
W1 C14 2.027(7) . ?
W1 C13 2.041(8) . ?
W1 C16 2.042(7) . ?
W1 P2 2.4170(16) . ?
W1 P1 2.4340(16) . ?
C6 N4 1.336(8) . ?
C6 C7 1.404(9) . ?
C6 C8 1.487(8) . ?
N3 N4 1.373(7) . ?
N3 P2 1.687(5) . ?
N3 Si1 1.758(5) . ?
Si1 N1 1.756(5) . ?
Si1 C11 1.832(7) . ?
Si1 C12 1.838(7) . ?
P2 C7 1.673(6) . ?
P1 C2 1.683(7) . ?
P1 N1 1.687(5) . ?
C7 C10 1.516(9) . ?
O4 C16 1.145(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N2 C1 1.317(8) . ?
N2 N1 1.384(7) . ?
C9 C8 1.513(10) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
O3 C15 1.141(8) . ?
C1 C2 1.431(9) . ?
C1 C3 1.501(8) . ?
O2 C14 1.113(8) . ?
C2 C5 1.507(9) . ?
C4 C3 1.509(10) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O1 C13 1.134(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 W1 C14 90.4(3) . . ?
C15 W1 C13 92.3(3) . . ?
C14 W1 C13 84.3(3) . . ?
C15 W1 C16 86.0(3) . . ?
C14 W1 C16 92.0(2) . . ?
C13 W1 C16 175.9(3) . . ?
C15 W1 P2 175.1(2) . . ?
C14 W1 P2 90.91(18) . . ?
C13 W1 P2 92.6(2) . . ?
C16 W1 P2 89.21(19) . . ?
C15 W1 P1 92.51(19) . . ?
C14 W1 P1 171.17(18) . . ?
C13 W1 P1 87.2(2) . . ?
C16 W1 P1 96.55(18) . . ?
P2 W1 P1 86.90(5) . . ?
N4 C6 C7 115.9(5) . . ?
N4 C6 C8 117.7(6) . . ?
C7 C6 C8 126.4(6) . . ?
N4 N3 P2 112.9(4) . . ?
N4 N3 Si1 112.1(4) . . ?
P2 N3 Si1 134.8(3) . . ?
N3 Si1 N1 105.4(2) . . ?
N3 Si1 C11 108.4(3) . . ?
N1 Si1 C11 108.7(3) . . ?
N3 Si1 C12 109.9(3) . . ?
N1 Si1 C12 108.7(3) . . ?
C11 Si1 C12 115.4(4) . . ?
C7 P2 N3 92.2(3) . . ?
C7 P2 W1 139.9(2) . . ?
N3 P2 W1 127.86(18) . . ?
C2 P1 N1 92.9(3) . . ?
C2 P1 W1 139.9(2) . . ?
N1 P1 W1 125.42(19) . . ?
C6 C7 C10 124.6(6) . . ?
C6 C7 P2 108.9(5) . . ?
C10 C7 P2 126.5(5) . . ?
C6 N4 N3 110.1(5) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C1 N2 N1 110.1(5) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 N1 P1 112.8(4) . . ?
N2 N1 Si1 109.7(4) . . ?
P1 N1 Si1 137.2(3) . . ?
C6 C8 C9 112.4(6) . . ?
C6 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
C6 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
N2 C1 C2 117.0(6) . . ?
N2 C1 C3 119.7(6) . . ?
C2 C1 C3 123.3(6) . . ?
C1 C2 C5 124.3(6) . . ?
C1 C2 P1 107.2(5) . . ?
C5 C2 P1 128.5(5) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C3 C4 114.6(6) . . ?
C1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
C1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C15 W1 177.9(7) . . ?
O2 C14 W1 175.9(6) . . ?
O1 C13 W1 177.2(7) . . ?
O4 C16 W1 177.7(6) . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         1.583
_refine_diff_density_min         -3.133
_refine_diff_density_rms         0.197

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_me180531Br1_13
_database_code_depnum_ccdc_archive 'CCDC 1920918'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H18 Br2 N4 Ni P2'
_chemical_formula_sum            'C10 H18 Br2 N4 Ni P2'
_chemical_formula_weight         474.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   29.0070(14)
_cell_length_b                   8.7064(3)
_cell_length_c                   14.4253(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.572(2)
_cell_angle_gamma                90
_cell_volume                     3473.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    27800
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_F_000             1872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.125
_exptl_absorpt_coefficient_mu    5.896
_shelx_estimated_absorpt_T_min   0.195
_shelx_estimated_absorpt_T_max   0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2603
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.349
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            27800
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.453
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3985
_reflns_number_gt                3337
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0364P)²+5.7328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3985
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0823
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.67280(2) 0.39731(4) 0.67660(2) 0.02426(10) Uani 1 1 d . . . . .
H1 H 0.5917(17) 0.558(5) 0.674(3) 0.042(13) Uiso 1 1 d . . . . .
C1 C 0.70737(12) 0.9261(4) 0.5034(3) 0.0239(7) Uani 1 1 d . . . . .
Ni1 Ni 0.63593(2) 0.50597(4) 0.52126(3) 0.01489(10) Uani 1 1 d . . . . .
P1 P 0.70442(4) 0.86790(10) 0.38821(7) 0.0264(2) Uani 1 1 d . . . . .
N1 N 0.66908(9) 0.6921(3) 0.49351(18) 0.0161(5) Uani 1 1 d . . . . .
P2 P 0.51830(3) 0.68007(11) 0.63461(6) 0.0249(2) Uani 1 1 d . . . . .
H2 H 0.6647(15) 0.636(4) 0.362(3) 0.032(11) Uiso 1 1 d . . . . .
Br2 Br 0.62110(2) 0.35957(4) 0.37648(2) 0.02437(10) Uani 1 1 d . . . . .
C2 C 0.68626(11) 0.8153(3) 0.5488(2) 0.0169(6) Uani 1 1 d . . . . .
N2 N 0.67647(10) 0.7081(3) 0.40542(19) 0.0198(6) Uani 1 1 d . . . . .
N3 N 0.57685(10) 0.6042(3) 0.53846(18) 0.0154(5) Uani 1 1 d . . . . .
C3 C 0.73013(15) 1.0723(4) 0.5515(3) 0.0358(9) Uani 1 1 d . . . . .
H3A H 0.7491 1.1190 0.5130 0.054 Uiso 1 1 calc R U . . .
H3B H 0.7514 1.0495 0.6170 0.054 Uiso 1 1 calc R U . . .
H3C H 0.7048 1.1438 0.5558 0.054 Uiso 1 1 calc R U . . .
N4 N 0.56890(11) 0.5977(3) 0.62644(19) 0.0188(6) Uani 1 1 d . . . . .
C4 C 0.68124(13) 0.8290(4) 0.6489(2) 0.0218(7) Uani 1 1 d . . . . .
H4A H 0.7115 0.8719 0.6934 0.026 Uiso 1 1 calc R U . . .
H4B H 0.6764 0.7256 0.6729 0.026 Uiso 1 1 calc R U . . .
C7 C 0.54063(12) 0.6800(3) 0.4755(2) 0.0160(6) Uani 1 1 d . . . . .
C6 C 0.50403(12) 0.7301(4) 0.5143(2) 0.0198(7) Uani 1 1 d . . . . .
C5 C 0.63881(14) 0.9320(4) 0.6502(3) 0.0294(8) Uani 1 1 d . . . . .
H5A H 0.6449 1.0369 0.6323 0.044 Uiso 1 1 calc R U . . .
H5B H 0.6352 0.9322 0.7156 0.044 Uiso 1 1 calc R U . . .
H5C H 0.6091 0.8930 0.6036 0.044 Uiso 1 1 calc R U . . .
C9 C 0.54131(13) 0.7087(4) 0.3738(2) 0.0233(7) Uani 1 1 d . . . . .
H9A H 0.5085 0.6907 0.3286 0.028 Uiso 1 1 calc R U . . .
H9B H 0.5635 0.6343 0.3576 0.028 Uiso 1 1 calc R U . . .
C8 C 0.45874(13) 0.8120(4) 0.4568(3) 0.0278(8) Uani 1 1 d . . . . .
H8A H 0.4671 0.9143 0.4385 0.042 Uiso 1 1 calc R U . . .
H8B H 0.4368 0.8220 0.4964 0.042 Uiso 1 1 calc R U . . .
H8C H 0.4429 0.7530 0.3979 0.042 Uiso 1 1 calc R U . . .
C10 C 0.55731(15) 0.8713(4) 0.3585(3) 0.0301(8) Uani 1 1 d . . . . .
H10A H 0.5597 0.8809 0.2924 0.045 Uiso 1 1 calc R U . . .
H10B H 0.5889 0.8922 0.4057 0.045 Uiso 1 1 calc R U . . .
H10C H 0.5336 0.9453 0.3676 0.045 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ni1 2.3692(5) . ?
C1 C2 1.405(4) . ?
C1 C3 1.504(5) . ?
C1 P1 1.715(4) . ?
Ni1 N1 1.986(3) . ?
Ni1 N3 1.997(3) . ?
Ni1 Br2 2.3727(5) . ?
P1 N2 1.666(3) . ?
N1 C2 1.340(4) . ?
N1 N2 1.358(3) . ?
P2 N4 1.669(3) . ?
P2 C6 1.714(3) . ?
C2 C4 1.500(4) . ?
N2 H2 0.88(4) . ?
N3 C7 1.337(4) . ?
N3 N4 1.358(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N4 H1 0.87(5) . ?
C4 C5 1.527(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 C6 1.411(4) . ?
C7 C9 1.495(4) . ?
C6 C8 1.505(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C9 C10 1.527(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C3 124.0(3) . . ?
C2 C1 P1 110.3(2) . . ?
C3 C1 P1 125.7(3) . . ?
N1 Ni1 N3 99.29(10) . . ?
N1 Ni1 Br1 114.13(8) . . ?
N3 Ni1 Br1 102.29(7) . . ?
N1 Ni1 Br2 103.36(7) . . ?
N3 Ni1 Br2 113.91(7) . . ?
Br1 Ni1 Br2 121.88(2) . . ?
N2 P1 C1 89.22(15) . . ?
C2 N1 N2 109.8(3) . . ?
C2 N1 Ni1 130.5(2) . . ?
N2 N1 Ni1 119.7(2) . . ?
N4 P2 C6 89.23(15) . . ?
N1 C2 C1 114.1(3) . . ?
N1 C2 C4 120.7(3) . . ?
C1 C2 C4 125.2(3) . . ?
N1 N2 P1 116.5(2) . . ?
N1 N2 H2 117(3) . . ?
P1 N2 H2 126(3) . . ?
C7 N3 N4 109.6(3) . . ?
C7 N3 Ni1 130.9(2) . . ?
N4 N3 Ni1 119.5(2) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 N4 P2 116.7(2) . . ?
N3 N4 H1 117(3) . . ?
P2 N4 H1 127(3) . . ?
C2 C4 C5 111.8(3) . . ?
C2 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
C2 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
N3 C7 C6 114.5(3) . . ?
N3 C7 C9 120.6(3) . . ?
C6 C7 C9 124.9(3) . . ?
C7 C6 C8 124.3(3) . . ?
C7 C6 P2 110.0(2) . . ?
C8 C6 P2 125.6(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C9 C10 113.1(3) . . ?
C7 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C7 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         0.525
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.137

