# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1009r2
_database_code_depnum_ccdc_archive 'CCDC 1453473'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[NbBr4(DMPE)2]]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 Br4 Nb P4'
_chemical_formula_sum            'C12 H32 Br4 Nb P4'
_chemical_formula_weight         712.80

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'
P P 0.1023 0.0942 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_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, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   13.3974(9)
_cell_length_b                   12.4285(9)
_cell_length_c                   14.1808(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2361.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20103
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_F_000             1380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    7.543
_shelx_estimated_absorpt_T_min   0.660
_shelx_estimated_absorpt_T_max   0.805
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            18564
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.657
_diffrn_reflns_theta_max         26.000
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4641
_reflns_number_gt                4406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0153P)²] 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_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.023(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4641
_refine_ls_number_parameters     199
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0435
_refine_ls_wR_factor_gt          0.0424
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Nb1 Nb 0.01192(3) 0.26101(4) 0.90660(3) 0.01199(10) Uani 1 1 d . . . . .
Br1 Br -0.16463(4) 0.26372(5) 0.81519(4) 0.02072(13) Uani 1 1 d . . . . .
Br2 Br -0.04859(4) 0.06782(4) 0.97462(4) 0.01687(12) Uani 1 1 d . . . . .
Br3 Br 0.12270(4) 0.34160(4) 1.04800(4) 0.01888(12) Uani 1 1 d . . . . .
Br4 Br 0.13848(4) 0.36635(5) 0.79168(4) 0.01995(13) Uani 1 1 d . . . . .
P1 P -0.11626(11) 0.29485(11) 1.05107(9) 0.0160(3) Uani 1 1 d . . . . .
P2 P -0.04352(11) 0.46895(12) 0.89902(10) 0.0197(3) Uani 1 1 d . . . . .
P3 P 0.02811(11) 0.13989(12) 0.74953(9) 0.0178(3) Uani 1 1 d . . . . .
P4 P 0.17655(10) 0.13837(12) 0.92447(10) 0.0148(3) Uani 1 1 d . . . . .
C1 C -0.0826(5) 0.2441(5) 1.1686(3) 0.0225(14) Uani 1 1 d . . . . .
H1A H -0.1307 0.2706 1.2151 0.034 Uiso 1 1 calc R U . . .
H1B H -0.0156 0.2694 1.1852 0.034 Uiso 1 1 calc R U . . .
H1C H -0.0835 0.1652 1.1681 0.034 Uiso 1 1 calc R U . . .
C2 C -0.2439(4) 0.2452(5) 1.0403(4) 0.0227(13) Uani 1 1 d . . . . .
H2A H -0.2781 0.2523 1.1011 0.034 Uiso 1 1 calc R U . . .
H2B H -0.2427 0.1693 1.0216 0.034 Uiso 1 1 calc R U . . .
H2C H -0.2795 0.2872 0.9924 0.034 Uiso 1 1 calc R U . . .
C3 C -0.1364(5) 0.4394(5) 1.0708(4) 0.0225(13) Uani 1 1 d . . . . .
H3A H -0.1959 0.4503 1.1112 0.027 Uiso 1 1 calc R U . . .
H3B H -0.0779 0.4708 1.1034 0.027 Uiso 1 1 calc R U . . .
C4 C -0.1518(4) 0.4954(5) 0.9756(4) 0.0244(13) Uani 1 1 d . . . . .
H4A H -0.1595 0.5738 0.9853 0.029 Uiso 1 1 calc R U . . .
H4B H -0.2134 0.4680 0.9453 0.029 Uiso 1 1 calc R U . . .
C5 C -0.0824(5) 0.5231(5) 0.7848(4) 0.0291(15) Uani 1 1 d . . . . .
H5A H -0.1392 0.4816 0.7610 0.044 Uiso 1 1 calc R U . . .
H5B H -0.0269 0.5182 0.7401 0.044 Uiso 1 1 calc R U . . .
H5C H -0.1021 0.5986 0.7923 0.044 Uiso 1 1 calc R U . . .
C6 C 0.0451(5) 0.5723(5) 0.9382(4) 0.0301(16) Uani 1 1 d . . . . .
H6A H 0.1066 0.5669 0.9011 0.045 Uiso 1 1 calc R U . . .
H6B H 0.0606 0.5613 1.0051 0.045 Uiso 1 1 calc R U . . .
H6C H 0.0155 0.6437 0.9295 0.045 Uiso 1 1 calc R U . . .
C7 C 0.0166(5) 0.2058(5) 0.6345(4) 0.0299(15) Uani 1 1 d . . . . .
H7A H 0.0150 0.1511 0.5847 0.045 Uiso 1 1 calc R U . . .
H7B H 0.0738 0.2536 0.6245 0.045 Uiso 1 1 calc R U . . .
H7C H -0.0452 0.2479 0.6327 0.045 Uiso 1 1 calc R U . . .
C8 C -0.0560(5) 0.0250(5) 0.7355(4) 0.0274(14) Uani 1 1 d . . . . .
H8A H -0.1246 0.0508 0.7277 0.041 Uiso 1 1 calc R U . . .
H8B H -0.0520 -0.0210 0.7915 0.041 Uiso 1 1 calc R U . . .
H8C H -0.0364 -0.0165 0.6797 0.041 Uiso 1 1 calc R U . . .
C9 C 0.1504(4) 0.0734(5) 0.7421(4) 0.0204(13) Uani 1 1 d . . . . .
H9A H 0.1479 0.0146 0.6951 0.024 Uiso 1 1 calc R U . . .
H9B H 0.2017 0.1258 0.7218 0.024 Uiso 1 1 calc R U . . .
C10 C 0.1773(4) 0.0280(4) 0.8389(3) 0.0189(12) Uani 1 1 d . . . . .
H10A H 0.2443 -0.0056 0.8367 0.023 Uiso 1 1 calc R U . . .
H10B H 0.1283 -0.0276 0.8576 0.023 Uiso 1 1 calc R U . . .
C11 C 0.1968(4) 0.0707(5) 1.0369(4) 0.0240(13) Uani 1 1 d . . . . .
H11A H 0.1467 0.0141 1.0451 0.036 Uiso 1 1 calc R U . . .
H11B H 0.1910 0.1230 1.0883 0.036 Uiso 1 1 calc R U . . .
H11C H 0.2636 0.0387 1.0377 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2991(4) 0.1988(4) 0.9043(4) 0.0218(12) Uani 1 1 d . . . . .
H12A H 0.3087 0.2590 0.9481 0.033 Uiso 1 1 calc R U . . .
H12B H 0.3030 0.2252 0.8393 0.033 Uiso 1 1 calc R U . . .
H12C H 0.3511 0.1447 0.9148 0.033 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
Nb1 Br3 2.6883(7) . ?
Nb1 P2 2.6912(16) . ?
Nb1 Br4 2.6916(7) . ?
Nb1 P4 2.6929(15) . ?
Nb1 P3 2.6970(15) . ?
Nb1 Br1 2.6975(7) . ?
Nb1 P1 2.7062(15) . ?
Nb1 Br2 2.7116(7) . ?
P1 C2 1.824(6) . ?
P1 C1 1.838(5) . ?
P1 C3 1.839(6) . ?
P2 C5 1.829(5) . ?
P2 C6 1.835(6) . ?
P2 C4 1.842(6) . ?
P3 C8 1.830(6) . ?
P3 C7 1.832(6) . ?
P3 C9 1.838(6) . ?
P4 C11 1.823(5) . ?
P4 C12 1.828(5) . ?
P4 C10 1.831(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.532(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
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 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.527(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
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
Br3 Nb1 P2 79.88(4) . . ?
Br3 Nb1 Br4 85.56(2) . . ?
P2 Nb1 Br4 71.49(3) . . ?
Br3 Nb1 P4 71.85(3) . . ?
P2 Nb1 P4 140.66(5) . . ?
Br4 Nb1 P4 79.42(4) . . ?
Br3 Nb1 P3 141.22(4) . . ?
P2 Nb1 P3 121.68(5) . . ?
Br4 Nb1 P3 73.79(4) . . ?
P4 Nb1 P3 72.30(4) . . ?
Br3 Nb1 Br1 146.92(2) . . ?
P2 Nb1 Br1 74.14(4) . . ?
Br4 Nb1 Br1 104.80(2) . . ?
P4 Nb1 Br1 140.40(4) . . ?
P3 Nb1 Br1 71.38(4) . . ?
Br3 Nb1 P1 74.20(3) . . ?
P2 Nb1 P1 72.89(4) . . ?
Br4 Nb1 P1 141.49(4) . . ?
P4 Nb1 P1 122.44(5) . . ?
P3 Nb1 P1 139.73(5) . . ?
Br1 Nb1 P1 78.78(4) . . ?
Br3 Nb1 Br2 103.28(2) . . ?
P2 Nb1 Br2 141.45(4) . . ?
Br4 Nb1 Br2 146.55(2) . . ?
P4 Nb1 Br2 73.15(3) . . ?
P3 Nb1 Br2 79.84(4) . . ?
Br1 Nb1 Br2 85.40(2) . . ?
P1 Nb1 Br2 71.25(3) . . ?
C2 P1 C1 101.0(3) . . ?
C2 P1 C3 101.9(3) . . ?
C1 P1 C3 103.5(3) . . ?
C2 P1 Nb1 118.60(18) . . ?
C1 P1 Nb1 118.5(2) . . ?
C3 P1 Nb1 111.12(18) . . ?
C5 P2 C6 101.2(3) . . ?
C5 P2 C4 103.4(3) . . ?
C6 P2 C4 101.9(3) . . ?
C5 P2 Nb1 117.9(2) . . ?
C6 P2 Nb1 118.8(2) . . ?
C4 P2 Nb1 111.41(19) . . ?
C8 P3 C7 101.5(3) . . ?
C8 P3 C9 101.1(3) . . ?
C7 P3 C9 103.0(3) . . ?
C8 P3 Nb1 118.42(19) . . ?
C7 P3 Nb1 118.6(2) . . ?
C9 P3 Nb1 111.71(18) . . ?
C11 P4 C12 101.1(3) . . ?
C11 P4 C10 103.5(3) . . ?
C12 P4 C10 101.5(3) . . ?
C11 P4 Nb1 117.73(19) . . ?
C12 P4 Nb1 119.21(18) . . ?
C10 P4 Nb1 111.47(19) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 109.2(4) . . ?
C4 C3 H3A 109.8 . . ?
P1 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
P1 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
C3 C4 P2 109.4(4) . . ?
C3 C4 H4A 109.8 . . ?
P2 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
P2 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P3 C7 H7A 109.5 . . ?
P3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P3 C8 H8A 109.5 . . ?
P3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P3 109.0(4) . . ?
C10 C9 H9A 109.9 . . ?
P3 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
P3 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 P4 108.5(4) . . ?
C9 C10 H10A 110.0 . . ?
P4 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
P4 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
P4 C11 H11A 109.5 . . ?
P4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P4 C12 H12A 109.5 . . ?
P4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         0.432
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.081

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1453474'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT222_shelx               
;
PROBLEM:	Large Non-Solvent  H     Uiso(max)/Uiso(min)
RESPONSE: These alerts are generated because there is a disorder carbon chain 
in the structure 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 Cl4 Nb P4'
_chemical_formula_sum            'C20 H48 Cl4 Nb P4'
_chemical_formula_weight         647.17

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   10.5571(5)
_cell_length_b                   11.6652(5)
_cell_length_c                   11.9053(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.008(7)
_cell_angle_gamma                90
_cell_volume                     1460.55(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13285
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             674
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.005
_shelx_estimated_absorpt_T_min   0.933
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            12265
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.028
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_point_group_measured_fraction_full 0.851
_reflns_number_total             4819
_reflns_number_gt                4748
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.597
_reflns_Friedel_fraction_max     0.661
_reflns_Friedel_fraction_full    0.688

_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0170P)²+0.5735P] 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_abs_structure_details 
; 
 Flack x determined using 1758 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.039(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4819
_refine_ls_number_parameters     280
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0402
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
Nb1 Nb 0.24668(2) 0.88419(2) 0.26926(2) 0.00786(6) Uani 1 1 d . . . . .
Cl1 Cl 0.05310(6) 0.95379(6) 0.35934(5) 0.01401(14) Uani 1 1 d . . . . .
Cl2 Cl 0.37989(6) 0.95755(6) 0.44047(5) 0.01333(14) Uani 1 1 d . . . . .
Cl3 Cl 0.39192(6) 0.92684(6) 0.11662(5) 0.01573(15) Uani 1 1 d . . . . .
Cl4 Cl 0.16435(6) 0.70996(6) 0.16035(5) 0.01178(13) Uani 1 1 d . . . . .
P1 P 0.07933(7) 0.94956(6) 0.09886(6) 0.01091(15) Uani 1 1 d . . . . .
P2 P 0.27052(7) 1.11180(7) 0.25016(6) 0.01238(15) Uani 1 1 d . . . . .
P3 P 0.19680(7) 0.73556(6) 0.43534(5) 0.01026(14) Uani 1 1 d . . . . .
P4 P 0.43808(7) 0.72854(6) 0.28681(6) 0.01116(15) Uani 1 1 d . . . . .
C1 C -0.0828(3) 0.8942(3) 0.1025(2) 0.0203(6) Uani 1 1 d . . . . .
H1A H -0.0854 0.8163 0.0695 0.024 Uiso 1 1 calc R U . . .
H1B H -0.1001 0.8862 0.1825 0.024 Uiso 1 1 calc R U . . .
C2 C -0.1902(3) 0.9632(3) 0.0428(3) 0.0304(8) Uani 1 1 d . . . . .
H2A H -0.1962 1.0377 0.0801 0.046 Uiso 1 1 calc R U . . .
H2B H -0.2704 0.9216 0.0458 0.046 Uiso 1 1 calc R U . . .
H2C H -0.1734 0.9751 -0.0360 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1230(3) 0.9123(3) -0.0425(2) 0.0240(8) Uani 1 1 d . . . . .
H3AA H 0.2170 0.9075 -0.0384 0.029 Uiso 0.5 1 calc R U P A 1
H3AB H 0.0900 0.8343 -0.0601 0.029 Uiso 0.5 1 calc R U P A 1
H3BC H 0.2074 0.9465 -0.0513 0.029 Uiso 0.5 1 calc R U P B 2
H3BD H 0.1335 0.8281 -0.0452 0.029 Uiso 0.5 1 calc R U P B 2
C5 C 0.1977(3) 1.1993(3) 0.3552(2) 0.0189(6) Uani 1 1 d . . . . .
H5A H 0.1047 1.1868 0.3454 0.023 Uiso 1 1 calc R U . . .
H5B H 0.2281 1.1702 0.4309 0.023 Uiso 1 1 calc R U . . .
C6 C 0.2217(4) 1.3287(3) 0.3539(3) 0.0306(8) Uani 1 1 d . . . . .
H6A H 0.3133 1.3434 0.3654 0.046 Uiso 1 1 calc R U . . .
H6B H 0.1789 1.3652 0.4143 0.046 Uiso 1 1 calc R U . . .
H6C H 0.1882 1.3603 0.2810 0.046 Uiso 1 1 calc R U . . .
C7 C 0.4346(3) 1.1667(3) 0.2561(3) 0.0198(6) Uani 1 1 d . . . . .
H7A H 0.4535 1.2059 0.3294 0.024 Uiso 1 1 calc R U . . .
H7B H 0.4928 1.1003 0.2548 0.024 Uiso 1 1 calc R U . . .
C8 C 0.4655(4) 1.2487(4) 0.1637(3) 0.0431(11) Uani 1 1 d . . . . .
H8A H 0.4551 1.2094 0.0908 0.065 Uiso 1 1 calc R U . . .
H8B H 0.5536 1.2751 0.1781 0.065 Uiso 1 1 calc R U . . .
H8C H 0.4079 1.3147 0.1626 0.065 Uiso 1 1 calc R U . . .
C9 C 0.0609(3) 1.1063(2) 0.0968(2) 0.0145(6) Uani 1 1 d . . . . .
H9A H 0.0185 1.1308 0.0233 0.017 Uiso 1 1 calc R U . . .
H9B H 0.0071 1.1302 0.1567 0.017 Uiso 1 1 calc R U . . .
C10 C 0.1911(3) 1.1630(3) 0.1158(2) 0.0151(6) Uani 1 1 d . . . . .
H10A H 0.1813 1.2474 0.1180 0.018 Uiso 1 1 calc R U . . .
H10B H 0.2431 1.1436 0.0531 0.018 Uiso 1 1 calc R U . . .
C11 C 0.0709(3) 0.6279(2) 0.4078(2) 0.0135(6) Uani 1 1 d . . . . .
H11A H 0.0964 0.5753 0.3486 0.016 Uiso 1 1 calc R U . . .
H11B H 0.0657 0.5821 0.4772 0.016 Uiso 1 1 calc R U . . .
C12 C -0.0617(3) 0.6740(3) 0.3710(2) 0.0182(6) Uani 1 1 d . . . . .
H12A H -0.0855 0.7317 0.4251 0.027 Uiso 1 1 calc R U . . .
H12B H -0.1232 0.6109 0.3680 0.027 Uiso 1 1 calc R U . . .
H12C H -0.0616 0.7090 0.2961 0.027 Uiso 1 1 calc R U . . .
C13 C 0.1628(3) 0.7965(3) 0.5723(2) 0.0165(6) Uani 1 1 d . . . . .
H13A H 0.2176 0.8645 0.5877 0.020 Uiso 1 1 calc R U . . .
H13B H 0.0734 0.8230 0.5665 0.020 Uiso 1 1 calc R U . . .
C14 C 0.1831(3) 0.7141(3) 0.6725(2) 0.0190(6) Uani 1 1 d . . . . .
H14A H 0.1301 0.6459 0.6580 0.029 Uiso 1 1 calc R U . . .
H14B H 0.1595 0.7524 0.7409 0.029 Uiso 1 1 calc R U . . .
H14C H 0.2728 0.6915 0.6827 0.029 Uiso 1 1 calc R U . . .
C15 C 0.5894(3) 0.7678(3) 0.3653(2) 0.0162(6) Uani 1 1 d . . . . .
H15A H 0.5720 0.7926 0.4420 0.019 Uiso 1 1 calc R U . . .
H15B H 0.6439 0.6988 0.3733 0.019 Uiso 1 1 calc R U . . .
C16 C 0.6629(3) 0.8631(3) 0.3110(3) 0.0230(7) Uani 1 1 d . . . . .
H16A H 0.6829 0.8388 0.2358 0.035 Uiso 1 1 calc R U . . .
H16B H 0.7420 0.8788 0.3579 0.035 Uiso 1 1 calc R U . . .
H16C H 0.6109 0.9328 0.3047 0.035 Uiso 1 1 calc R U . . .
C17 C 0.4861(3) 0.6653(3) 0.1560(2) 0.0186(6) Uani 1 1 d . . . . .
H17A H 0.4092 0.6347 0.1125 0.022 Uiso 1 1 calc R U . . .
H17B H 0.5206 0.7270 0.1104 0.022 Uiso 1 1 calc R U . . .
C18 C 0.5840(4) 0.5700(4) 0.1705(3) 0.0390(10) Uani 1 1 d . . . . .
H18A H 0.6648 0.6014 0.2040 0.059 Uiso 1 1 calc R U . . .
H18B H 0.5965 0.5365 0.0968 0.059 Uiso 1 1 calc R U . . .
H18C H 0.5541 0.5107 0.2201 0.059 Uiso 1 1 calc R U . . .
C19 C 0.3338(3) 0.6419(3) 0.4726(2) 0.0142(6) Uani 1 1 d . . . . .
H19A H 0.3983 0.6838 0.5220 0.017 Uiso 1 1 calc R U . . .
H19B H 0.3062 0.5742 0.5143 0.017 Uiso 1 1 calc R U . . .
C20 C 0.3919(3) 0.6028(3) 0.3659(2) 0.0143(6) Uani 1 1 d . . . . .
H20A H 0.3293 0.5565 0.3186 0.017 Uiso 1 1 calc R U . . .
H20B H 0.4675 0.5544 0.3864 0.017 Uiso 1 1 calc R U . . .
C4 C 0.0815(9) 0.9866(8) -0.1395(8) 0.026(2) Uani 0.5 1 d . . P C 1
H4A H -0.0103 1.0001 -0.1410 0.039 Uiso 0.5 1 calc R U P C 1
H4B H 0.1006 0.9490 -0.2096 0.039 Uiso 0.5 1 calc R U P C 1
H4C H 0.1266 1.0600 -0.1321 0.039 Uiso 0.5 1 calc R U P C 1
C4A C 0.0367(8) 0.9464(8) -0.1425(8) 0.0192(18) Uani 0.5 1 d . . P C 2
H4AA H -0.0440 0.9050 -0.1418 0.029 Uiso 0.5 1 calc R U P C 2
H4AB H 0.0765 0.9274 -0.2116 0.029 Uiso 0.5 1 calc R U P C 2
H4AC H 0.0208 1.0291 -0.1401 0.029 Uiso 0.5 1 calc R U P C 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
Nb1 Cl2 2.5228(7) . ?
Nb1 Cl1 2.5235(7) . ?
Nb1 Cl4 2.5240(7) . ?
Nb1 Cl3 2.5273(7) . ?
Nb1 P2 2.6785(8) . ?
Nb1 P1 2.6818(7) . ?
Nb1 P4 2.7111(7) . ?
Nb1 P3 2.7157(7) . ?
P1 C1 1.833(3) . ?
P1 C3 1.836(3) . ?
P1 C9 1.839(3) . ?
P2 C5 1.834(3) . ?
P2 C10 1.840(3) . ?
P2 C7 1.843(3) . ?
P3 C19 1.835(3) . ?
P3 C11 1.837(3) . ?
P3 C13 1.842(3) . ?
P4 C20 1.832(3) . ?
P4 C17 1.834(3) . ?
P4 C15 1.836(3) . ?
C1 C2 1.516(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.479(9) . ?
C3 C4A 1.489(9) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C5 C6 1.530(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.514(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.525(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.528(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.532(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.531(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.518(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.528(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 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
Cl2 Nb1 Cl1 87.85(2) . . ?
Cl2 Nb1 Cl4 146.19(2) . . ?
Cl1 Nb1 Cl4 102.83(2) . . ?
Cl2 Nb1 Cl3 100.59(2) . . ?
Cl1 Nb1 Cl3 143.79(2) . . ?
Cl4 Nb1 Cl3 89.57(2) . . ?
Cl2 Nb1 P2 71.49(2) . . ?
Cl1 Nb1 P2 78.62(2) . . ?
Cl4 Nb1 P2 141.75(2) . . ?
Cl3 Nb1 P2 71.12(2) . . ?
Cl2 Nb1 P1 143.01(2) . . ?
Cl1 Nb1 P1 74.07(2) . . ?
Cl4 Nb1 P1 70.48(2) . . ?
Cl3 Nb1 P1 78.53(2) . . ?
P2 Nb1 P1 73.41(2) . . ?
Cl2 Nb1 P4 78.80(2) . . ?
Cl1 Nb1 P4 143.95(2) . . ?
Cl4 Nb1 P4 73.81(2) . . ?
Cl3 Nb1 P4 72.08(2) . . ?
P2 Nb1 P4 126.55(2) . . ?
P1 Nb1 P4 133.32(2) . . ?
Cl2 Nb1 P3 76.00(2) . . ?
Cl1 Nb1 P3 71.36(2) . . ?
Cl4 Nb1 P3 77.29(2) . . ?
Cl3 Nb1 P3 144.84(2) . . ?
P2 Nb1 P3 136.08(2) . . ?
P1 Nb1 P3 125.13(2) . . ?
P4 Nb1 P3 72.95(2) . . ?
C1 P1 C3 104.38(15) . . ?
C1 P1 C9 104.62(15) . . ?
C3 P1 C9 104.95(14) . . ?
C1 P1 Nb1 115.88(9) . . ?
C3 P1 Nb1 115.13(10) . . ?
C9 P1 Nb1 110.78(9) . . ?
C5 P2 C10 103.05(14) . . ?
C5 P2 C7 103.23(15) . . ?
C10 P2 C7 106.00(13) . . ?
C5 P2 Nb1 116.48(10) . . ?
C10 P2 Nb1 110.90(10) . . ?
C7 P2 Nb1 115.88(11) . . ?
C19 P3 C11 100.29(13) . . ?
C19 P3 C13 103.08(13) . . ?
C11 P3 C13 103.15(13) . . ?
C19 P3 Nb1 110.92(9) . . ?
C11 P3 Nb1 119.33(9) . . ?
C13 P3 Nb1 117.60(10) . . ?
C20 P4 C17 102.68(14) . . ?
C20 P4 C15 101.37(13) . . ?
C17 P4 C15 103.88(14) . . ?
C20 P4 Nb1 110.25(9) . . ?
C17 P4 Nb1 117.60(10) . . ?
C15 P4 Nb1 118.77(10) . . ?
C2 C1 P1 117.6(2) . . ?
C2 C1 H1A 107.9 . . ?
P1 C1 H1A 107.9 . . ?
C2 C1 H1B 107.9 . . ?
P1 C1 H1B 107.9 . . ?
H1A C1 H1B 107.2 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 119.7(4) . . ?
C4A C3 P1 119.0(4) . . ?
C4 C3 H3AA 107.4 . . ?
P1 C3 H3AA 107.4 . . ?
C4 C3 H3AB 107.4 . . ?
P1 C3 H3AB 107.4 . . ?
H3AA C3 H3AB 106.9 . . ?
C4A C3 H3BC 107.6 . . ?
P1 C3 H3BC 107.6 . . ?
C4A C3 H3BD 107.6 . . ?
P1 C3 H3BD 107.6 . . ?
H3BC C3 H3BD 107.0 . . ?
C6 C5 P2 117.5(2) . . ?
C6 C5 H5A 107.9 . . ?
P2 C5 H5A 107.9 . . ?
C6 C5 H5B 107.9 . . ?
P2 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
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 . . ?
C8 C7 P2 117.0(2) . . ?
C8 C7 H7A 108.1 . . ?
P2 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
P2 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 109.67(19) . . ?
C10 C9 H9A 109.7 . . ?
P1 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
P1 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 P2 108.90(19) . . ?
C9 C10 H10A 109.9 . . ?
P2 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
P2 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 P3 116.2(2) . . ?
C12 C11 H11A 108.2 . . ?
P3 C11 H11A 108.2 . . ?
C12 C11 H11B 108.2 . . ?
P3 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
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 . . ?
C14 C13 P3 115.0(2) . . ?
C14 C13 H13A 108.5 . . ?
P3 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
P3 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 P4 114.7(2) . . ?
C16 C15 H15A 108.6 . . ?
P4 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
P4 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 P4 115.7(2) . . ?
C18 C17 H17A 108.3 . . ?
P4 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
P4 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
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 . . ?
C20 C19 P3 110.03(19) . . ?
C20 C19 H19A 109.7 . . ?
P3 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
P3 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C19 C20 P4 109.4(2) . . ?
C19 C20 H20A 109.8 . . ?
P4 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
P4 C20 H20B 109.8 . . ?
H20A C20 H20B 108.2 . . ?
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 . . ?
C3 C4A H4AA 109.5 . . ?
C3 C4A H4AB 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
C3 C4A H4AC 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?

_refine_diff_density_max         0.324
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.047

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1453475'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[NbCl4(o-DMPB)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 Cl4 Nb P4'
_chemical_formula_sum            'C20 H32 Cl4 Nb P4'
_chemical_formula_weight         631.04

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'

_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'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   8.9876(7)
_cell_length_b                   8.9876(7)
_cell_length_c                   16.1482(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1304.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2286
_cell_measurement_theta_min      4.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             642
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.124
_shelx_estimated_absorpt_T_min   0.915
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            2204
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.081
_diffrn_reflns_theta_max         26.941
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             754
_reflns_number_gt                703
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_max     0.929
_reflns_Friedel_fraction_full    0.955

_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0158P)²+13.9926P] 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_abs_structure_details 
; 
 Flack x determined using 263 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         754
_refine_ls_number_parameters     43
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
Nb1 Nb 0.0000 1.0000 1.0000 0.0327(6) Uani 1 8 d S T P . .
Cl1 Cl -0.1836(2) 0.8164(2) 0.95577(16) 0.0378(7) Uani 1 2 d S T P . .
P1 P 0.12483(19) 0.87517(19) 0.86449(13) 0.0161(5) Uani 1 2 d S T P . .
C1 C 0.1007(9) 0.6750(8) 0.8545(4) 0.0308(17) Uani 1 1 d . . . . .
H1A H -0.0053 0.6520 0.8483 0.046 Uiso 1 1 calc R U . . .
H1B H 0.1394 0.6256 0.9041 0.046 Uiso 1 1 calc R U . . .
H1C H 0.1549 0.6395 0.8057 0.046 Uiso 1 1 calc R U . . .
C2 C 0.0546(7) 0.9454(7) 0.7655(5) 0.0164(17) Uani 1 2 d S T P . .
C3 C 0.1098(8) 0.8902(8) 0.6895(5) 0.0209(19) Uani 1 2 d S T P . .
H3 H 0.1846 0.8154 0.6889 0.025 Uiso 1 2 calc R U P . .
C4 C 0.0536(9) 0.9464(9) 0.6159(5) 0.024(2) Uani 1 2 d S T P . .
H4 H 0.0904 0.9096 0.5647 0.029 Uiso 1 2 calc R U P . .


_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
Nb1 Cl1 2.441(3) . ?
Nb1 Cl1 2.441(3) 2_575 ?
Nb1 Cl1 2.441(3) 4_667 ?
Nb1 Cl1 2.441(3) 3_467 ?
Nb1 P1 2.703(2) 4_667 ?
Nb1 P1 2.703(2) 2_575 ?
Nb1 P1 2.703(2) 3_467 ?
Nb1 P1 2.703(2) . ?
P1 C1 1.819(8) 7_665 ?
P1 C1 1.819(8) . ?
P1 C2 1.831(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C2 1.388(19) 2_575 ?
C2 C3 1.414(12) . ?
C3 C4 1.388(13) . ?
C3 H3 0.9500 . ?
C4 C4 1.36(2) 2_575 ?
C4 H4 0.9500 . ?

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
Cl1 Nb1 Cl1 145.97(13) . 2_575 ?
Cl1 Nb1 Cl1 94.91(4) . 4_667 ?
Cl1 Nb1 Cl1 94.91(4) 2_575 4_667 ?
Cl1 Nb1 Cl1 94.91(4) . 3_467 ?
Cl1 Nb1 Cl1 94.91(4) 2_575 3_467 ?
Cl1 Nb1 Cl1 145.97(13) 4_667 3_467 ?
Cl1 Nb1 P1 142.96(8) . 4_667 ?
Cl1 Nb1 P1 71.07(8) 2_575 4_667 ?
Cl1 Nb1 P1 76.30(5) 4_667 4_667 ?
Cl1 Nb1 P1 76.30(5) 3_467 4_667 ?
Cl1 Nb1 P1 76.30(5) . 2_575 ?
Cl1 Nb1 P1 76.30(5) 2_575 2_575 ?
Cl1 Nb1 P1 142.96(8) 4_667 2_575 ?
Cl1 Nb1 P1 71.07(8) 3_467 2_575 ?
P1 Nb1 P1 130.95(6) 4_667 2_575 ?
Cl1 Nb1 P1 71.07(8) . 3_467 ?
Cl1 Nb1 P1 142.96(8) 2_575 3_467 ?
Cl1 Nb1 P1 76.30(5) 4_667 3_467 ?
Cl1 Nb1 P1 76.30(5) 3_467 3_467 ?
P1 Nb1 P1 71.89(10) 4_667 3_467 ?
P1 Nb1 P1 130.95(6) 2_575 3_467 ?
Cl1 Nb1 P1 76.30(5) . . ?
Cl1 Nb1 P1 76.30(5) 2_575 . ?
Cl1 Nb1 P1 71.07(8) 4_667 . ?
Cl1 Nb1 P1 142.96(8) 3_467 . ?
P1 Nb1 P1 130.95(6) 4_667 . ?
P1 Nb1 P1 71.89(10) 2_575 . ?
P1 Nb1 P1 130.95(6) 3_467 . ?
C1 P1 C1 103.2(5) 7_665 . ?
C1 P1 C2 102.9(3) 7_665 . ?
C1 P1 C2 102.9(3) . . ?
C1 P1 Nb1 115.6(2) 7_665 . ?
C1 P1 Nb1 115.6(2) . . ?
C2 P1 Nb1 114.9(3) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C2 C3 119.8(6) 2_575 . ?
C2 C2 P1 119.2(3) 2_575 . ?
C3 C2 P1 121.0(7) . . ?
C4 C3 C2 119.2(9) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C4 C4 C3 121.0(6) 2_575 . ?
C4 C4 H4 119.5 2_575 . ?
C3 C4 H4 119.5 . . ?

_refine_diff_density_max         1.380
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.118

####################################################################### 
# 
# 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_140515ypc1
_database_code_depnum_ccdc_archive 'CCDC 1453476'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[NbCl4(DMPE)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 Cl4 Nb P4'
_chemical_formula_sum            'C12 H32 Cl4 Nb P4'
_chemical_formula_weight         534.96

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

_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'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.7216(9)
_cell_length_b                   11.2891(10)
_cell_length_c                   9.4711(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1146.36(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10275
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             546
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            9661
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.390
_diffrn_reflns_theta_max         25.982
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2248
_reflns_number_gt                2167
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_max     1.001
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0152P)²+0.4233P]
 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_abs_structure_details 
;
 Flack x determined using 894 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.05(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2248
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0457
_refine_ls_wR_factor_gt          0.0453
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Nb1 Nb 0.0000 1.0000 0.25811(4) 0.01021(10) Uani 1 2 d S T P . .
Cl1 Cl 0.15158(7) 1.10373(7) 0.09626(9) 0.01711(18) Uani 1 1 d . . . . .
Cl2 Cl 0.03076(7) 1.17450(7) 0.42025(8) 0.01809(19) Uani 1 1 d . . . . .
P1 P 0.12143(8) 0.83178(7) 0.11847(9) 0.01428(18) Uani 1 1 d . . . . .
P2 P 0.21607(7) 0.97105(7) 0.39133(9) 0.01506(19) Uani 1 1 d . . . . .
C1 C 0.3354(3) 1.0850(3) 0.3669(4) 0.0228(8) Uani 1 1 d . . . . .
H1A H 0.4027 1.0729 0.4354 0.034 Uiso 1 1 calc R U . . .
H1B H 0.2983 1.1634 0.3813 0.034 Uiso 1 1 calc R U . . .
H1C H 0.3692 1.0798 0.2710 0.034 Uiso 1 1 calc R U . . .
C2 C 0.2104(3) 0.9574(3) 0.5824(3) 0.0240(8) Uani 1 1 d . . . . .
H2A H 0.1493 0.8967 0.6086 0.036 Uiso 1 1 calc R U . . .
H2B H 0.1861 1.0335 0.6239 0.036 Uiso 1 1 calc R U . . .
H2C H 0.2929 0.9346 0.6179 0.036 Uiso 1 1 calc R U . . .
C3 C 0.2951(3) 0.8362(3) 0.3320(3) 0.0191(8) Uani 1 1 d . . . . .
H3A H 0.3838 0.8386 0.3609 0.023 Uiso 1 1 calc R U . . .
H3B H 0.2559 0.7661 0.3765 0.023 Uiso 1 1 calc R U . . .
C4 C 0.2862(3) 0.8262(3) 0.1714(3) 0.0190(7) Uani 1 1 d . . . . .
H4A H 0.3238 0.7506 0.1398 0.023 Uiso 1 1 calc R U . . .
H4B H 0.3325 0.8921 0.1266 0.023 Uiso 1 1 calc R U . . .
C5 C 0.0710(3) 0.6787(3) 0.1416(4) 0.0238(8) Uani 1 1 d . . . . .
H5A H -0.0189 0.6730 0.1238 0.036 Uiso 1 1 calc R U . . .
H5B H 0.0888 0.6532 0.2384 0.036 Uiso 1 1 calc R U . . .
H5C H 0.1159 0.6277 0.0751 0.036 Uiso 1 1 calc R U . . .
C6 C 0.1261(3) 0.8470(3) -0.0727(3) 0.0218(8) Uani 1 1 d . . . . .
H6A H 0.1787 0.7844 -0.1128 0.033 Uiso 1 1 calc R U . . .
H6B H 0.1607 0.9246 -0.0975 0.033 Uiso 1 1 calc R U . . .
H6C H 0.0414 0.8400 -0.1108 0.033 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
Nb1 Cl2 2.5194(8) 2_575 ?
Nb1 Cl2 2.5195(8) . ?
Nb1 Cl1 2.5224(8) 2_575 ?
Nb1 Cl1 2.5224(8) . ?
Nb1 P1 2.6553(8) 2_575 ?
Nb1 P1 2.6553(8) . ?
Nb1 P2 2.6580(8) 2_575 ?
Nb1 P2 2.6581(8) . ?
P1 C6 1.820(3) . ?
P1 C5 1.824(4) . ?
P1 C4 1.837(3) . ?
P2 C2 1.817(3) . ?
P2 C1 1.829(3) . ?
P2 C3 1.831(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.529(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 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
Cl2 Nb1 Cl2 104.89(4) 2_575 . ?
Cl2 Nb1 Cl1 85.59(3) 2_575 2_575 ?
Cl2 Nb1 Cl1 144.86(2) . 2_575 ?
Cl2 Nb1 Cl1 144.86(2) 2_575 . ?
Cl2 Nb1 Cl1 85.59(3) . . ?
Cl1 Nb1 Cl1 105.15(4) 2_575 . ?
Cl2 Nb1 P1 143.00(2) 2_575 2_575 ?
Cl2 Nb1 P1 78.96(3) . 2_575 ?
Cl1 Nb1 P1 73.35(3) 2_575 2_575 ?
Cl1 Nb1 P1 71.41(3) . 2_575 ?
Cl2 Nb1 P1 78.96(3) 2_575 . ?
Cl2 Nb1 P1 143.00(2) . . ?
Cl1 Nb1 P1 71.41(3) 2_575 . ?
Cl1 Nb1 P1 73.35(3) . . ?
P1 Nb1 P1 120.25(4) 2_575 . ?
Cl2 Nb1 P2 72.10(2) 2_575 2_575 ?
Cl2 Nb1 P2 74.25(2) . 2_575 ?
Cl1 Nb1 P2 77.53(3) 2_575 2_575 ?
Cl1 Nb1 P2 142.46(2) . 2_575 ?
P1 Nb1 P2 73.81(3) 2_575 2_575 ?
P1 Nb1 P2 138.74(3) . 2_575 ?
Cl2 Nb1 P2 74.26(2) 2_575 . ?
Cl2 Nb1 P2 72.11(2) . . ?
Cl1 Nb1 P2 142.46(2) 2_575 . ?
Cl1 Nb1 P2 77.53(3) . . ?
P1 Nb1 P2 138.74(3) 2_575 . ?
P1 Nb1 P2 73.81(3) . . ?
P2 Nb1 P2 123.32(4) 2_575 . ?
C6 P1 C5 102.53(16) . . ?
C6 P1 C4 104.38(16) . . ?
C5 P1 C4 102.69(17) . . ?
C6 P1 Nb1 116.22(12) . . ?
C5 P1 Nb1 118.18(11) . . ?
C4 P1 Nb1 111.11(12) . . ?
C2 P2 C1 102.04(16) . . ?
C2 P2 C3 104.50(16) . . ?
C1 P2 C3 102.85(17) . . ?
C2 P2 Nb1 117.01(12) . . ?
C1 P2 Nb1 117.60(12) . . ?
C3 P2 Nb1 111.10(11) . . ?
P2 C1 H1A 109.5 . . ?
P2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P2 C2 H2A 109.5 . . ?
P2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P2 109.7(3) . . ?
C4 C3 H3A 109.7 . . ?
P2 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
P2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 P1 109.2(2) . . ?
C3 C4 H4A 109.8 . . ?
P1 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
P1 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
P1 C5 H5A 109.5 . . ?
P1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P1 C6 H6A 109.5 . . ?
P1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_refine_diff_density_max         0.263
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.057

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_2015_0606r3
_database_code_depnum_ccdc_archive 'CCDC 1453477'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[{NbOCl3(DEPE)2}(DEPE)]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H72 Cl6 Nb2 O2 P6'
_chemical_formula_sum            'C30 H72 Cl6 Nb2 O2 P6'
_chemical_formula_weight         1049.21

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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                   9.8162(3)
_cell_length_b                   11.6449(3)
_cell_length_c                   20.2185(14)
_cell_angle_alpha                90
_cell_angle_beta                 95.496(7)
_cell_angle_gamma                90
_cell_volume                     2300.52(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17854
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Column
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_F_000             1084
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.082
_shelx_estimated_absorpt_T_min   0.863
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            20644
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.042
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5247
_reflns_number_gt                4591
_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0245P)²+2.3917P] 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         5247
_refine_ls_number_parameters     214
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.073
_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
Nb1 Nb 0.21947(2) 0.20723(2) 0.11474(2) 0.01321(6) Uani 1 1 d . U . . .
Cl1 Cl 0.10248(6) 0.06239(5) 0.18058(3) 0.02252(13) Uani 1 1 d . . . . .
Cl2 Cl 0.43888(6) 0.18235(5) 0.19424(3) 0.02053(12) Uani 1 1 d . . . . .
Cl3 Cl 0.36831(6) 0.23311(5) 0.02394(3) 0.02226(13) Uani 1 1 d . . . . .
O1 O 0.07385(16) 0.25770(14) 0.06960(8) 0.0189(3) Uani 1 1 d . . . . .
P1 P 0.13046(6) 0.30369(5) 0.22420(3) 0.01533(12) Uani 1 1 d . . . . .
P2 P 0.31048(6) 0.42305(5) 0.12649(3) 0.01566(12) Uani 1 1 d . . . . .
P3 P 0.21288(6) -0.00222(5) 0.05033(3) 0.01488(11) Uani 1 1 d . U . . .
C1 C -0.0561(2) 0.3004(2) 0.22644(12) 0.0217(5) Uani 1 1 d . . . . .
H1A H -0.0870 0.2194 0.2236 0.026 Uiso 1 1 calc R U . . .
H1B H -0.0783 0.3309 0.2698 0.026 Uiso 1 1 calc R U . . .
C2 C -0.1365(3) 0.3686(2) 0.17123(13) 0.0275(5) Uani 1 1 d . . . . .
H2A H -0.1105 0.4498 0.1749 0.041 Uiso 1 1 calc R U . . .
H2B H -0.2348 0.3608 0.1754 0.041 Uiso 1 1 calc R U . . .
H2C H -0.1159 0.3390 0.1279 0.041 Uiso 1 1 calc R U . . .
C3 C 0.2036(2) 0.2369(2) 0.30211(11) 0.0200(5) Uani 1 1 d . . . . .
H3A H 0.2165 0.1540 0.2940 0.024 Uiso 1 1 calc R U . . .
H3B H 0.2952 0.2706 0.3143 0.024 Uiso 1 1 calc R U . . .
C4 C 0.1189(3) 0.2503(3) 0.36091(12) 0.0323(6) Uani 1 1 d . . . . .
H4A H 0.0926 0.3310 0.3651 0.049 Uiso 1 1 calc R U . . .
H4B H 0.1731 0.2257 0.4017 0.049 Uiso 1 1 calc R U . . .
H4C H 0.0364 0.2028 0.3538 0.049 Uiso 1 1 calc R U . . .
C5 C 0.4795(3) 0.4547(2) 0.10153(13) 0.0238(5) Uani 1 1 d . . . . .
H5A H 0.5460 0.4013 0.1251 0.029 Uiso 1 1 calc R U . . .
H5B H 0.4789 0.4392 0.0534 0.029 Uiso 1 1 calc R U . . .
C6 C 0.5293(3) 0.5770(2) 0.11484(14) 0.0351(7) Uani 1 1 d . . . . .
H6A H 0.4656 0.6309 0.0910 0.053 Uiso 1 1 calc R U . . .
H6B H 0.6204 0.5862 0.0995 0.053 Uiso 1 1 calc R U . . .
H6C H 0.5341 0.5927 0.1626 0.053 Uiso 1 1 calc R U . . .
C7 C 0.1918(3) 0.5249(2) 0.08191(12) 0.0233(5) Uani 1 1 d . . . . .
H7A H 0.0982 0.5090 0.0940 0.028 Uiso 1 1 calc R U . . .
H7B H 0.2166 0.6035 0.0973 0.028 Uiso 1 1 calc R U . . .
C8 C 0.1895(3) 0.5215(2) 0.00664(13) 0.0310(6) Uani 1 1 d . . . . .
H8A H 0.2801 0.5420 -0.0062 0.047 Uiso 1 1 calc R U . . .
H8B H 0.1215 0.5764 -0.0130 0.047 Uiso 1 1 calc R U . . .
H8C H 0.1654 0.4440 -0.0093 0.047 Uiso 1 1 calc R U . . .
C9 C 0.1777(3) 0.45493(19) 0.23808(12) 0.0209(5) Uani 1 1 d . . . . .
H9A H 0.1077 0.5053 0.2145 0.025 Uiso 1 1 calc R U . . .
H9B H 0.1828 0.4729 0.2861 0.025 Uiso 1 1 calc R U . . .
C10 C 0.3157(3) 0.4758(2) 0.21222(11) 0.0212(5) Uani 1 1 d . . . . .
H10A H 0.3881 0.4351 0.2405 0.025 Uiso 1 1 calc R U . . .
H10B H 0.3370 0.5589 0.2136 0.025 Uiso 1 1 calc R U . . .
C11 C 0.2942(2) -0.0192(2) -0.02704(12) 0.0210(5) Uani 1 1 d . . . . .
H11A H 0.2661 0.0462 -0.0565 0.025 Uiso 1 1 calc R U . . .
H11B H 0.3946 -0.0138 -0.0163 0.025 Uiso 1 1 calc R U . . .
C12 C 0.2633(3) -0.1303(2) -0.06596(13) 0.0288(6) Uani 1 1 d . . . . .
H12A H 0.2891 -0.1963 -0.0374 0.043 Uiso 1 1 calc R U . . .
H12B H 0.3157 -0.1317 -0.1048 0.043 Uiso 1 1 calc R U . . .
H12C H 0.1653 -0.1340 -0.0806 0.043 Uiso 1 1 calc R U . . .
C13 C 0.2756(2) -0.1262(2) 0.10039(12) 0.0217(5) Uani 1 1 d . . . . .
H13A H 0.2200 -0.1342 0.1384 0.026 Uiso 1 1 calc R U . . .
H13B H 0.2621 -0.1965 0.0730 0.026 Uiso 1 1 calc R U . . .
C14 C 0.4259(3) -0.1181(2) 0.12684(15) 0.0326(6) Uani 1 1 d . . . . .
H14A H 0.4831 -0.1247 0.0898 0.049 Uiso 1 1 calc R U . . .
H14B H 0.4484 -0.1804 0.1586 0.049 Uiso 1 1 calc R U . . .
H14C H 0.4430 -0.0440 0.1491 0.049 Uiso 1 1 calc R U . . .
C15 C 0.0342(2) -0.04037(19) 0.02672(11) 0.0165(4) Uani 1 1 d . . . . .
H15A H 0.0297 -0.1201 0.0097 0.020 Uiso 1 1 calc R U . . .
H15B H -0.0171 -0.0373 0.0665 0.020 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
Nb1 O1 1.7239(16) . ?
Nb1 Cl3 2.4717(6) . ?
Nb1 Cl1 2.4956(6) . ?
Nb1 Cl2 2.5774(6) . ?
Nb1 P2 2.6703(6) . ?
Nb1 P1 2.7007(6) . ?
Nb1 P3 2.7627(6) . ?
P1 C9 1.836(2) . ?
P1 C1 1.837(2) . ?
P1 C3 1.840(2) . ?
P2 C5 1.818(2) . ?
P2 C10 1.835(2) . ?
P2 C7 1.837(2) . ?
P3 C15 1.828(2) . ?
P3 C11 1.834(2) . ?
P3 C13 1.836(2) . ?
C1 C2 1.527(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.523(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.522(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.520(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.518(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.529(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.523(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C15 1.537(4) 3 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?

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
O1 Nb1 Cl3 94.84(6) . . ?
O1 Nb1 Cl1 96.44(6) . . ?
Cl3 Nb1 Cl1 144.44(2) . . ?
O1 Nb1 Cl2 165.81(5) . . ?
Cl3 Nb1 Cl2 87.64(2) . . ?
Cl1 Nb1 Cl2 89.49(2) . . ?
O1 Nb1 P2 88.83(5) . . ?
Cl3 Nb1 P2 74.621(18) . . ?
Cl1 Nb1 P2 139.092(19) . . ?
Cl2 Nb1 P2 78.337(19) . . ?
O1 Nb1 P1 88.57(5) . . ?
Cl3 Nb1 P1 144.942(19) . . ?
Cl1 Nb1 P1 69.054(18) . . ?
Cl2 Nb1 P1 81.511(18) . . ?
P2 Nb1 P1 70.570(18) . . ?
O1 Nb1 P3 94.05(5) . . ?
Cl3 Nb1 P3 75.307(18) . . ?
Cl1 Nb1 P3 70.342(18) . . ?
Cl2 Nb1 P3 100.089(19) . . ?
P2 Nb1 P3 149.926(19) . . ?
P1 Nb1 P3 139.348(18) . . ?
C9 P1 C1 104.72(11) . . ?
C9 P1 C3 101.68(11) . . ?
C1 P1 C3 106.18(11) . . ?
C9 P1 Nb1 115.31(8) . . ?
C1 P1 Nb1 114.40(8) . . ?
C3 P1 Nb1 113.28(8) . . ?
C5 P2 C10 104.53(11) . . ?
C5 P2 C7 106.61(12) . . ?
C10 P2 C7 101.92(11) . . ?
C5 P2 Nb1 118.20(8) . . ?
C10 P2 Nb1 112.19(8) . . ?
C7 P2 Nb1 111.89(8) . . ?
C15 P3 C11 103.67(10) . . ?
C15 P3 C13 102.46(10) . . ?
C11 P3 C13 103.58(11) . . ?
C15 P3 Nb1 108.43(7) . . ?
C11 P3 Nb1 120.33(8) . . ?
C13 P3 Nb1 116.30(8) . . ?
C2 C1 P1 114.71(17) . . ?
C2 C1 H1A 108.6 . . ?
P1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
P1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 115.30(17) . . ?
C4 C3 H3A 108.4 . . ?
P1 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
P1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
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 . . ?
C6 C5 P2 115.27(18) . . ?
C6 C5 H5A 108.5 . . ?
P2 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
P2 C5 H5B 108.5 . . ?
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 . . ?
C8 C7 P2 114.98(18) . . ?
C8 C7 H7A 108.5 . . ?
P2 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
P2 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 108.75(16) . . ?
C10 C9 H9A 109.9 . . ?
P1 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
P1 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 P2 109.08(16) . . ?
C9 C10 H10A 109.9 . . ?
P2 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
P2 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 P3 116.68(17) . . ?
C12 C11 H11A 108.1 . . ?
P3 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
P3 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
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 . . ?
C14 C13 P3 114.03(17) . . ?
C14 C13 H13A 108.7 . . ?
P3 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
P3 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C15 P3 112.2(2) 3 . ?
C15 C15 H15A 109.2 3 . ?
P3 C15 H15A 109.2 . . ?
C15 C15 H15B 109.2 3 . ?
P3 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?

_refine_diff_density_max         0.502
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.080

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1453478'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ 
RESPONSE:  The CH3 group on acetonitrile is located at
	special position. Therefre, the Hydrogens do not be added.
	This also causes PLAT043 and PLAT068.
;
# end Validation Reply Form



_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 H32 Br4 Nb P4, C2 H3 Br4 N Nb O'
_chemical_formula_sum            'C14 H35 Br8 N Nb2 O P4'
_chemical_formula_weight         1182.41

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'

_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'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   12.011(3)
_cell_length_b                   12.011(3)
_cell_length_c                   11.065(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1596.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9842
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chunk
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    10.942
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            10587
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.392
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1835
_reflns_number_gt                1758
_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0188P)²+2.7440P] 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         1835
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0188
_refine_ls_wR_factor_ref         0.0490
_refine_ls_wR_factor_gt          0.0486
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
Nb1 Nb 0.7500 0.2500 0.5000 0.00529(9) Uani 1 4 d S T P . .
Br1 Br 0.94288(2) 0.17314(2) 0.43301(2) 0.01028(7) Uani 1 1 d . . . . .
P1 P 0.87604(5) 0.21023(5) 0.69826(5) 0.00785(12) Uani 1 1 d . . . . .
C1 C 1.0150(2) 0.2712(2) 0.7029(2) 0.0147(5) Uani 1 1 d . . . . .
H1A H 1.0380 0.2810 0.7872 0.022 Uiso 1 1 calc R U . . .
H1B H 1.0140 0.3437 0.6623 0.022 Uiso 1 1 calc R U . . .
H1C H 1.0676 0.2217 0.6618 0.022 Uiso 1 1 calc R U . . .
C2 C 0.9017(2) 0.0648(2) 0.7348(2) 0.0142(5) Uani 1 1 d . . . . .
H2A H 0.9285 0.0258 0.6627 0.021 Uiso 1 1 calc R U . . .
H2B H 0.8324 0.0303 0.7628 0.021 Uiso 1 1 calc R U . . .
H2C H 0.9580 0.0601 0.7987 0.021 Uiso 1 1 calc R U . . .
C3 C 0.81181(19) 0.2645(2) 0.8359(2) 0.0124(5) Uani 1 1 d . . . . .
H3A H 0.8482 0.2314 0.9077 0.015 Uiso 1 1 calc R U . . .
H3B H 0.8214 0.3463 0.8396 0.015 Uiso 1 1 calc R U . . .
Nb2 Nb 0.2500 0.2500 0.00311(3) 0.00795(9) Uani 1 4 d S T P . .
Br2 Br 0.06204(2) 0.15483(2) 0.03408(2) 0.01639(8) Uani 1 1 d . . . . .
N1 N 0.2500 0.2500 0.2237(4) 0.0161(8) Uani 1 4 d S T P . .
O1 O 0.2500 0.2500 -0.1504(3) 0.0116(6) Uani 1 4 d S T P . .
C4 C 0.2500 0.2500 0.3270(4) 0.0134(9) Uani 1 4 d S T P . .
C5 C 0.2500 0.2500 0.4585(4) 0.0202(11) Uani 1 4 d S T P . .


_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
Nb1 Br1 2.6017(6) . ?
Nb1 Br1 2.6017(6) 8_656 ?
Nb1 Br1 2.6017(6) 7_666 ?
Nb1 Br1 2.6017(6) 2_655 ?
Nb1 P1 2.7079(9) . ?
Nb1 P1 2.7079(9) 7_666 ?
Nb1 P1 2.7079(9) 2_655 ?
Nb1 P1 2.7079(9) 8_656 ?
P1 C2 1.819(2) . ?
P1 C1 1.823(3) . ?
P1 C3 1.827(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C3 1.525(5) 2_655 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
Nb2 O1 1.699(3) . ?
Nb2 N1 2.441(4) . ?
Nb2 Br2 2.5535(7) . ?
Nb2 Br2 2.5536(7) 2 ?
Nb2 Br2 2.5536(7) 4 ?
Nb2 Br2 2.5536(7) 3 ?
N1 C4 1.142(6) . ?
C4 C5 1.455(6) . ?

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
Br1 Nb1 Br1 94.656(4) . 8_656 ?
Br1 Nb1 Br1 94.656(5) . 7_666 ?
Br1 Nb1 Br1 146.895(17) 8_656 7_666 ?
Br1 Nb1 Br1 146.894(17) . 2_655 ?
Br1 Nb1 Br1 94.655(4) 8_656 2_655 ?
Br1 Nb1 Br1 94.655(4) 7_666 2_655 ?
Br1 Nb1 P1 70.76(2) . . ?
Br1 Nb1 P1 74.210(15) 8_656 . ?
Br1 Nb1 P1 79.076(16) 7_666 . ?
Br1 Nb1 P1 142.300(14) 2_655 . ?
Br1 Nb1 P1 74.209(15) . 7_666 ?
Br1 Nb1 P1 142.301(14) 8_656 7_666 ?
Br1 Nb1 P1 70.75(2) 7_666 7_666 ?
Br1 Nb1 P1 79.077(15) 2_655 7_666 ?
P1 Nb1 P1 131.02(2) . 7_666 ?
Br1 Nb1 P1 142.302(14) . 2_655 ?
Br1 Nb1 P1 79.077(16) 8_656 2_655 ?
Br1 Nb1 P1 74.210(15) 7_666 2_655 ?
Br1 Nb1 P1 70.75(2) 2_655 2_655 ?
P1 Nb1 P1 71.78(3) . 2_655 ?
P1 Nb1 P1 131.02(2) 7_666 2_655 ?
Br1 Nb1 P1 79.077(16) . 8_656 ?
Br1 Nb1 P1 70.75(2) 8_656 8_656 ?
Br1 Nb1 P1 142.301(14) 7_666 8_656 ?
Br1 Nb1 P1 74.210(14) 2_655 8_656 ?
P1 Nb1 P1 131.02(2) . 8_656 ?
P1 Nb1 P1 71.78(3) 7_666 8_656 ?
P1 Nb1 P1 131.02(2) 2_655 8_656 ?
C2 P1 C1 102.98(12) . . ?
C2 P1 C3 103.20(11) . . ?
C1 P1 C3 102.68(11) . . ?
C2 P1 Nb1 116.37(8) . . ?
C1 P1 Nb1 117.64(8) . . ?
C3 P1 Nb1 112.10(8) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C3 P1 109.26(12) 2_655 . ?
C3 C3 H3A 109.8 2_655 . ?
P1 C3 H3A 109.8 . . ?
C3 C3 H3B 109.8 2_655 . ?
P1 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
O1 Nb2 N1 180.0 . . ?
O1 Nb2 Br2 97.711(11) . . ?
N1 Nb2 Br2 82.289(11) . . ?
O1 Nb2 Br2 97.712(11) . 2 ?
N1 Nb2 Br2 82.288(11) . 2 ?
Br2 Nb2 Br2 164.58(2) . 2 ?
O1 Nb2 Br2 97.712(11) . 4 ?
N1 Nb2 Br2 82.288(11) . 4 ?
Br2 Nb2 Br2 88.968(3) . 4 ?
Br2 Nb2 Br2 88.968(3) 2 4 ?
O1 Nb2 Br2 97.712(11) . 3 ?
N1 Nb2 Br2 82.288(11) . 3 ?
Br2 Nb2 Br2 88.969(3) . 3 ?
Br2 Nb2 Br2 88.968(3) 2 3 ?
Br2 Nb2 Br2 164.58(2) 4 3 ?
C4 N1 Nb2 180.0 . . ?
N1 C4 C5 180.0 . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.110

####################################################################### 
# 
# 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_NBBR4_2_publ
_database_code_depnum_ccdc_archive 'CCDC 1453489'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT021_NBBR4_2_publ        
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      1.645    
RESPONSE: This is Powder diffraction refinement. Therefore,
 refinement with redundant (i.e. not merged/unique) data set. 
;
# end Validation Reply Form


_pd_block_id                     2016-02-09T10:29|NBBR4_2|YP_Chang|D2_phaser

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2016-02-09T10:29

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
; ?
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  GSAS

_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    none

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               0
_pd_prep_pressure                100
_pd_prep_temperature             298

_pd_char_colour                  Brown
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     22
_refine_ls_goodness_of_fit_all   3.31
_refine_ls_number_restraints     0
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        'Niobium(IV) Tetrabromoide'
_chemical_name_common            'Niobium(IV) Tetrabromoide'
_chemical_formula_moiety         'Br4 Nb'
_chemical_formula_structural     'Br4 Nb'
_chemical_formula_analytical     'Br4 Nb'
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  '-I 2y'

_exptl_crystal_F_000             724
_exptl_crystal_density_diffrn    4.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS


_pd_phase_name                   'from C:/GSAS/MyWork/NbCl4.cif'
_cell_length_a                   8.6119(6)
_cell_length_b                   7.1821(5)
_cell_length_c                   9.3626(8)
_cell_angle_alpha                90.0
_cell_angle_beta                 92.212(4)
_cell_angle_gamma                90.0
_cell_volume                     578.65(9)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 1 2/m 1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z
-1 -x,-y,-z
-2 +x,-y,+z
101 +x+1/2,+y+1/2,+z+1/2
102 -x+1/2,+y+1/2,-z+1/2
-101 -x+1/2,-y+1/2,-z+1/2
-102 +x+1/2,-y+1/2,+z+1/2

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Nb Nb1 0.0 0.2168(7) 0.0 1.0 Uiso 0.0154(12) 4
Br Br1 0.0399(7) 0.0 0.2175(7) 1.0 Uiso 0.0285(23) 4
Br Br2 -0.27946(29) 0.2649(7) 0.02692(28) 1.0 Uiso 0.0246(11) 8
Br Br3 0.0261(7) 0.5 0.1951(6) 1.0 Uiso 0.0130(17) 4

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'Br4 Nb'
_chemical_formula_weight         412.52
_cell_formula_units_Z            4

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Nb1 3.114(10) . -1_555 N
Nb1 Br1 2.575(6) . 1_555 N
Nb1 Br1 2.575(6) . 2_555 N
Nb1 Br2 2.4540(25) . 1_555 N
Nb1 Br2 2.4540(25) . 2_555 N
Nb1 Br3 2.738(6) . 1_555 N
Nb1 Br3 2.738(6) . 2_555 N
Br1 Nb1 2.575(6) . 1_555 N
Br1 Nb1 2.575(6) . -1_555 N
Br1 Br3 3.5988(9) . 1_545 N
Br1 Br3 3.5988(9) . 1_555 N
Br2 Nb1 2.4540(25) . 1_555 N
Br2 Br2 3.377(10) . -2_565 N
Br2 Br3 3.455(6) . 1_555 N
Br2 Br3 3.505(6) . 2_555 N
Br3 Nb1 2.738(6) . 1_555 N
Br3 Nb1 2.738(6) . -1_565 N
Br3 Br1 3.5988(9) . 1_555 N
Br3 Br1 3.5988(9) . 1_565 N
Br3 Br2 3.455(6) . 1_555 N
Br3 Br2 3.505(6) . 2_555 N
Br3 Br2 3.505(6) . -1_565 N
Br3 Br2 3.455(6) . -2_565 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Nb1 Br1 105.62(26) 1_555 . 2_555 N
Br1 Nb1 Br2 96.04(14) 1_555 . 1_555 N
Br1 Nb1 Br2 93.73(15) 1_555 . 2_555 N
Br1 Nb1 Br3 85.21(8) 1_555 . 1_555 N
Br1 Nb1 Br3 169.03(23) 1_555 . 2_555 N
Br1 Nb1 Br2 93.73(15) 2_555 . 1_555 N
Br1 Nb1 Br2 96.04(14) 2_555 . 2_555 N
Br1 Nb1 Br3 169.03(23) 2_555 . 1_555 N
Br1 Nb1 Br3 85.21(8) 2_555 . 2_555 N
Br2 Nb1 Br2 163.81(19) 1_555 . 2_555 N
Br2 Nb1 Br3 83.24(14) 1_555 . 1_555 N
Br2 Nb1 Br3 84.74(15) 1_555 . 2_555 N
Br2 Nb1 Br3 84.74(15) 2_555 . 1_555 N
Br2 Nb1 Br3 83.24(14) 2_555 . 2_555 N
Br3 Nb1 Br3 84.02(22) 1_555 . 2_555 N
Nb1 Br1 Nb1 74.38(26) 1_555 . -1_555 N
Nb1 Br3 Nb1 95.98(22) 1_555 . -1_565 N

# Powder diffraction data for histogram  1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_measurement_device_type  'Bruker D2 Phaser'
_diffrn_detector                 '1D LYNXEYE'
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       'DIFFRAC.SUITE COMMANDER'
_computing_data_reduction        'PowDLL Converter'

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  none

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              5

_pd_spec_size_equat              5

_pd_spec_size_thick              1

_pd_spec_mounting                'Aluminium plate'


_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder


loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Nb 4.0 0.000 0.000 17.6142 1.18865 12.0144 11.7660 4.04183 0.20479 3.53346
69.7957 3.75591 International_Tables_Vol_C
Br-1 16.0 0.000 0.000 17.1718 2.20590 6.33380 19.3345 5.57540 0.28710 3.72720
58.1535 3.17760 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.7


_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_pd_proc_ls_prof_R_factor        0.0270
_pd_proc_ls_prof_wR_factor       0.0371
_pd_proc_ls_prof_wR_expected     0.0113
_refine_ls_R_Fsqd_factor         0.04651

_pd_proc_ls_background_function  
;   GSAS Background function number 1 with 36 terms.
 Shifted Chebyshev function of 1st kind
      1:    5633.33     2:   -262.308     3:   -573.988     4:    372.446    
      5:    433.322     6:   -555.263     7:    415.686     8:   -2.09579    
      9:   -136.286    10:    250.245    11:    64.5635    12:   -136.380    
     13:    45.9897    14:    80.3626    15:   -1.43480    16:   -154.686    
     17:    97.8114    18:   -165.955    19:    182.124    20:   -141.059    
     21:    76.1504    22:   -11.9297    23:    73.8984    24:   -102.286    
     25:    9.91100    26:    31.3136    27:   -69.7405    28:    75.5684    
     29:   -145.760    30:    168.715    31:   -174.654    32:    98.8768    
     33:   -55.8614    34:    101.608    35:   -128.550    36:    96.4285    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
# Extinction correction
_gsas_exptl_extinct_corr_T_min   1.00000
_gsas_exptl_extinct_corr_T_max   1.00000

_pd_proc_ls_profile_function     
;
 CW Profile function number 2 with  18 terms
 Profile coefficients for Simpson's rule integration of pseudovoigt function
 C.J. Howard (1982). J. Appl. Cryst.,15,615-620.
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 #1(GU)   =  882.863 #2(GV)   = -161.687 #3(GW)   =   23.032
 #4(LX)   =   30.179 #5(LY)   =    1.000 #6(trns) =    0.000
 #7(asym) =   0.0000 #8(shft) =   0.0000 #9(GP)   =    0.000
 #10(stec)=     0.00 #11(ptec)=     0.00 #12(sfec)=     0.00
 #13(L11) =    0.000 #14(L22) =    0.000 #15(L33) =    0.000
 #16(L12) =    0.000 #17(L13) =    0.000 #18(L23) =    0.000
 Peak tails are ignored  where the intensity is below 0.0001 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff          0.00010
_pd_proc_info_datetime           2016-02-09T10:29:39
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        13.002
_pd_meas_2theta_range_max        84.99538
_pd_meas_2theta_range_inc        0.02026
_pd_proc_2theta_range_min        12.86698
_pd_proc_2theta_range_max        84.86036
_pd_proc_2theta_range_inc        0.02026

loop_
_pd_meas_counts_total
_pd_proc_ls_weight
_pd_proc_intensity_bkg_calc
_pd_calc_intensity_total
7744.0 0.0001291 6002.93066 6760.84033
7568.0 0.0001321 6373.32666 7164.04688
7682.0 0.0001302 6648.37451 7474.14258
7446.0 0.0001343 6840.40381 7703.67627
7524.0 0.0001329 6960.61279 7864.07813
7594.0 0.0001317 7019.14844 7965.76318
7530.0 0.0001328 7025.23730 8018.25000
7379.0 0.0001355 6987.21582 8030.21729
7530.0 0.0001328 6912.58789 8009.55615
7485.0 0.0001336 6808.11816 7963.46289
7518.0 0.0001330 6679.86084 7898.48730
7545.0 0.0001325 6533.22461 7820.61523
7626.0 0.0001311 6372.98633 7735.29395
7636.0 0.0001310 6203.44678 7647.58105
7537.0 0.0001327 6028.33154 7562.11523
7596.0 0.0001316 5850.90332 7483.23193
7694.0 0.0001300 5674.02979 7415.06299
7625.0 0.0001311 5500.19092 7361.60547
7702.0 0.0001298 5331.47607 7326.78418
7759.0 0.0001289 5169.64600 7314.61230
7898.0 0.0001266 5016.20508 7329.20117
7875.0 0.0001270 4872.35938 7375.00586
7968.0 0.0001255 4739.08545 7456.91211
8024.0 0.0001246 4617.11035 7580.33838
8024.0 0.0001246 4507.01074 7751.34863
8329.0 0.0001201 4409.15234 7976.79639
8726.0 0.0001146 4323.75830 8264.43652
8816.0 0.0001134 4250.89160 8622.96191
9143.0 0.0001094 4190.52734 9061.81836
9491.0 0.0001054 4142.49902 9591.34668
9853.0 0.0001015 4106.55566 10222.36719
10496.0 0.0000953 4082.37158 10965.54688
11237.0 0.0000890 4069.54517 11830.43750
12274.0 0.0000815 4067.61377 12823.82422
13492.0 0.0000741 4076.06738 13946.78418
15333.0 0.0000652 4094.35596 15190.11328
16700.0 0.0000599 4121.89795 16528.31445
18280.0 0.0000547 4158.08154 17912.83984
19746.0 0.0000506 4202.28906 19266.54297
21239.0 0.0000471 4253.87549 20484.56445
21648.0 0.0000462 4312.20117 21447.12891
22033.0 0.0000454 4376.61816 22045.45508
21934.0 0.0000456 4446.49512 22212.74219
21602.0 0.0000463 4521.17822 21946.20117
20925.0 0.0000478 4600.05273 21307.69531
20556.0 0.0000486 4682.51416 20402.86523
19622.0 0.0000510 4767.96143 19353.85938
18292.0 0.0000547 4855.80811 18263.05469
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5941.0 0.0001683 5484.52002 6035.78320
5870.0 0.0001704 5486.11084 6048.96973
5868.0 0.0001704 5490.11328 6065.60596
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_pd_meas_number_of_points        3555
_pd_proc_number_of_points        3555

_reflns_number_total             380
_reflns_limit_h_min              0
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              7
_reflns_limit_l_min              -9
_reflns_limit_l_max              9
_reflns_d_resolution_high        1.201
_reflns_d_resolution_low         6.459
#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
