# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_3366

# Crystallographer: Michael R. Gau

# Compound 2

_database_code_depnum_ccdc_archive 'CCDC 1970109'
loop_
_audit_author_name
_audit_author_address
'Patrick Carroll'
;University of Pennsylvania
United States of America
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;

_audit_creation_date             2018-03-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_formula_moiety         'C43.4 H38.5 Cl0.1 N3 Ni O0.9 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C51.40 H54.50 Cl0.10 N3 Ni O2.90 P2'
_chemical_formula_weight         884.87

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5572(6)
_cell_length_b                   11.7407(6)
_cell_length_c                   16.9501(8)
_cell_angle_alpha                100.184(2)
_cell_angle_beta                 93.978(2)
_cell_angle_gamma                102.322(2)
_cell_volume                     2197.81(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.562
_cell_measurement_theta_min      3.214
_shelx_estimated_absorpt_T_max   0.920
_shelx_estimated_absorpt_T_min   0.871
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016/2'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58237
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         3.214
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                8500
_reflns_number_total             10118
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2016.1-0'
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'Mercury 4.2.0 (Macrae et al., 2008)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         10118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0280P)²+2.6989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0892
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.26344(2) 0.68902(2) 0.72694(2) 0.00929(6) Uani 1 1 d . . . . .
Cl1 Cl 0.2395(13) 0.4887(8) 0.7110(7) 0.025(3) Uani 0.1 1 d . . P A 2
P1 P 0.33798(4) 0.62415(4) 0.56177(3) 0.00887(10) Uani 1 1 d . . . . .
P2 P 0.34307(4) 0.63084(4) 0.89105(3) 0.00991(10) Uani 1 1 d . . . . .
O1 O 0.2627(3) 0.5267(2) 0.7077(2) 0.0111(6) Uani 0.9 1 d . . P A 1
O2 O 0.72549(15) 0.57822(15) 0.77261(11) 0.0321(4) Uani 1 1 d . . . . .
O3 O 0.61091(17) 0.90192(15) 0.68832(10) 0.0363(4) Uani 1 1 d . . . . .
N1 N 0.26328(14) 0.70214(14) 0.61695(9) 0.0111(3) Uani 1 1 d . . . . .
N2 N 0.23303(14) 0.83911(13) 0.74389(9) 0.0108(3) Uani 1 1 d . . . . .
N3 N 0.28198(14) 0.71154(13) 0.84146(9) 0.0109(3) Uani 1 1 d . . . . .
C1 C 0.22801(16) 0.80568(16) 0.60269(11) 0.0108(4) Uani 1 1 d . . . . .
C2 C 0.19836(17) 0.83025(17) 0.52754(11) 0.0132(4) Uani 1 1 d . . . . .
H2 H 0.200209 0.774237 0.480035 0.016 Uiso 1 1 calc R . . . .
C3 C 0.16595(18) 0.93635(18) 0.52134(12) 0.0166(4) Uani 1 1 d . . . . .
H3 H 0.145375 0.952495 0.469870 0.020 Uiso 1 1 calc R . . . .
C4 C 0.16394(18) 1.01813(18) 0.59077(12) 0.0174(4) Uani 1 1 d . . . . .
H4 H 0.145540 1.092086 0.586591 0.021 Uiso 1 1 calc R . . . .
C5 C 0.18861(17) 0.99298(17) 0.66659(12) 0.0149(4) Uani 1 1 d . . . . .
H5 H 0.187179 1.050170 0.713555 0.018 Uiso 1 1 calc R . . . .
C6 C 0.21561(16) 0.88407(16) 0.67452(11) 0.0109(4) Uani 1 1 d . . . . .
C7 C 0.20262(16) 0.87595(16) 0.82018(11) 0.0103(4) Uani 1 1 d . . . . .
C8 C 0.14421(16) 0.96658(16) 0.84750(12) 0.0125(4) Uani 1 1 d . . . . .
H8 H 0.122427 1.013739 0.811396 0.015 Uiso 1 1 calc R . . . .
C9 C 0.11797(17) 0.98784(17) 0.92707(12) 0.0140(4) Uani 1 1 d . . . . .
H9 H 0.078766 1.049690 0.944413 0.017 Uiso 1 1 calc R . . . .
C10 C 0.14780(17) 0.92087(17) 0.98117(12) 0.0140(4) Uani 1 1 d . . . . .
H10 H 0.131300 0.937811 1.035592 0.017 Uiso 1 1 calc R . . . .
C11 C 0.20253(16) 0.82789(16) 0.95497(11) 0.0121(4) Uani 1 1 d . . . . .
H11 H 0.220939 0.779757 0.991403 0.015 Uiso 1 1 calc R . . . .
C12 C 0.23031(16) 0.80513(16) 0.87604(11) 0.0104(4) Uani 1 1 d . . . . .
C13 C 0.39579(16) 0.69320(16) 0.48079(11) 0.0107(4) Uani 1 1 d . . . . .
C14 C 0.47243(17) 0.80636(17) 0.50051(12) 0.0142(4) Uani 1 1 d . . . . .
H14 H 0.488674 0.847620 0.555023 0.017 Uiso 1 1 calc R . . . .
C15 C 0.52450(18) 0.85798(18) 0.44029(13) 0.0178(4) Uani 1 1 d . . . . .
H15 H 0.576285 0.934867 0.453507 0.021 Uiso 1 1 calc R . . . .
C16 C 0.5011(2) 0.79747(19) 0.36063(13) 0.0233(5) Uani 1 1 d . . . . .
H16 H 0.537560 0.832747 0.319535 0.028 Uiso 1 1 calc R . . . .
C17 C 0.4249(2) 0.68596(19) 0.34096(12) 0.0214(4) Uani 1 1 d . . . . .
H17 H 0.408579 0.645137 0.286350 0.026 Uiso 1 1 calc R . . . .
C18 C 0.37205(17) 0.63357(17) 0.40090(11) 0.0136(4) Uani 1 1 d . . . . .
H18 H 0.319717 0.556993 0.387272 0.016 Uiso 1 1 calc R . . . .
C19 C 0.25175(16) 0.47724(16) 0.51706(11) 0.0111(4) Uani 1 1 d . . . . .
C20 C 0.13830(17) 0.46675(18) 0.47873(12) 0.0160(4) Uani 1 1 d . . . . .
H20 H 0.108775 0.535845 0.476644 0.019 Uiso 1 1 calc R . . . .
C21 C 0.06851(18) 0.35534(19) 0.44363(13) 0.0193(4) Uani 1 1 d . . . . .
H21 H -0.008982 0.348262 0.417731 0.023 Uiso 1 1 calc R . . . .
C22 C 0.11136(18) 0.25436(18) 0.44619(13) 0.0192(4) Uani 1 1 d . . . . .
H22 H 0.063118 0.178189 0.422302 0.023 Uiso 1 1 calc R . . . .
C23 C 0.22454(18) 0.26441(18) 0.48358(12) 0.0175(4) Uani 1 1 d . . . . .
H23 H 0.254302 0.195180 0.484576 0.021 Uiso 1 1 calc R . . . .
C24 C 0.29468(17) 0.37570(17) 0.51966(11) 0.0135(4) Uani 1 1 d . . . . .
H24 H 0.371780 0.382388 0.546038 0.016 Uiso 1 1 calc R . . . .
C25 C 0.47000(16) 0.60984(17) 0.61757(11) 0.0127(4) Uani 1 1 d . . . . .
H25a H 0.518581 0.689051 0.642028 0.019 Uiso 1 1 calc GR . . . .
H25b H 0.515907 0.567415 0.581140 0.019 Uiso 1 1 calc GR . . . .
H25c H 0.447668 0.565242 0.660042 0.019 Uiso 1 1 calc GR . . . .
C26 C 0.42203(16) 0.71558(17) 0.98626(11) 0.0118(4) Uani 1 1 d . . . . .
C27 C 0.41084(18) 0.67570(18) 1.05859(12) 0.0166(4) Uani 1 1 d . . . . .
H27 H 0.354614 0.604470 1.060405 0.020 Uiso 1 1 calc R . . . .
C28 C 0.4823(2) 0.7407(2) 1.12815(12) 0.0226(5) Uani 1 1 d . . . . .
H28 H 0.475378 0.713170 1.177449 0.027 Uiso 1 1 calc R . . . .
C29 C 0.56350(19) 0.8450(2) 1.12605(13) 0.0211(4) Uani 1 1 d . . . . .
H29 H 0.612518 0.888501 1.173741 0.025 Uiso 1 1 calc R . . . .
C30 C 0.57354(18) 0.88620(19) 1.05439(13) 0.0192(4) Uani 1 1 d . . . . .
H30 H 0.628702 0.958354 1.053095 0.023 Uiso 1 1 calc R . . . .
C31 C 0.50293(18) 0.82189(18) 0.98487(12) 0.0167(4) Uani 1 1 d . . . . .
H31 H 0.509555 0.850257 0.935863 0.020 Uiso 1 1 calc R . . . .
C32 C 0.23919(17) 0.50379(16) 0.91007(11) 0.0134(4) Uani 1 1 d . . . . .
C33 C 0.11840(19) 0.50261(18) 0.90220(13) 0.0203(4) Uani 1 1 d . . . . .
H33 H 0.092582 0.569386 0.889338 0.024 Uiso 1 1 calc R . . . .
C34 C 0.0355(2) 0.4036(2) 0.91319(15) 0.0267(5) Uani 1 1 d . . . . .
H34 H -0.047093 0.402723 0.908201 0.032 Uiso 1 1 calc R . . . .
C35 C 0.0734(2) 0.3063(2) 0.93139(15) 0.0286(5) Uani 1 1 d . . . . .
H35 H 0.016642 0.238972 0.939433 0.034 Uiso 1 1 calc R . . . .
C36 C 0.1934(2) 0.30616(19) 0.93798(15) 0.0267(5) Uani 1 1 d . . . . .
H36 H 0.218694 0.238460 0.949635 0.032 Uiso 1 1 calc R . . . .
C37 C 0.27684(19) 0.40495(18) 0.92756(13) 0.0210(4) Uani 1 1 d . . . . .
H37 H 0.359292 0.405246 0.932328 0.025 Uiso 1 1 calc R . . . .
C38 C 0.45761(18) 0.57777(18) 0.83976(12) 0.0166(4) Uani 1 1 d . . . . .
H38a H 0.421416 0.519509 0.790808 0.025 Uiso 1 1 calc GR . . . .
H38b H 0.501317 0.540137 0.875305 0.025 Uiso 1 1 calc GR . . . .
H38c H 0.512681 0.644651 0.825156 0.025 Uiso 1 1 calc GR . . . .
C39 C 0.1547(2) 0.4527(2) 0.70216(12) 0.0110(4) Uani 0.9 1 d . . P A 1
C40 C 0.1464(2) 0.33102(19) 0.69934(14) 0.0166(4) Uani 0.9 1 d . . P A 1
H40 H 0.216751 0.301521 0.700479 0.020 Uiso 0.9 1 calc R . P A 1
C41 C 0.0357(2) 0.2531(2) 0.69487(15) 0.0219(5) Uani 0.9 1 d . . P A 1
H41 H 0.031579 0.171111 0.693682 0.026 Uiso 0.9 1 calc R . P A 1
C42 C -0.0682(2) 0.2935(2) 0.69215(14) 0.0206(5) Uani 0.9 1 d . . P A 1
H42 H -0.143495 0.239825 0.688446 0.025 Uiso 0.9 1 calc R . P A 1
C43 C -0.0608(2) 0.4130(2) 0.69489(14) 0.0206(5) Uani 0.9 1 d . . P A 1
H43 H -0.131557 0.441834 0.693335 0.025 Uiso 0.9 1 calc R . P A 1
C44 C 0.0489(2) 0.4916(2) 0.69989(14) 0.0168(5) Uani 0.9 1 d . . P A 1
H44 H 0.052018 0.573569 0.701806 0.020 Uiso 0.9 1 calc R . P A 1
C45 C 0.8022(3) 0.6003(2) 0.84572(16) 0.0386(6) Uani 1 1 d . . . . .
H45a H 0.856935 0.545712 0.841601 0.046 Uiso 1 1 calc R . . . .
H45b H 0.754864 0.587812 0.891233 0.046 Uiso 1 1 calc R . . . .
C46 C 0.8725(2) 0.7287(2) 0.85929(16) 0.0361(6) Uani 1 1 d . . . . .
H46a H 0.832434 0.782785 0.893107 0.043 Uiso 1 1 calc R . . . .
H46b H 0.954415 0.737786 0.885005 0.043 Uiso 1 1 calc R . . . .
C47 C 0.8735(2) 0.7521(2) 0.77396(15) 0.0319(5) Uani 1 1 d . . . . .
H47a H 0.881563 0.837652 0.773420 0.038 Uiso 1 1 calc R . . . .
H47b H 0.938585 0.724393 0.747067 0.038 Uiso 1 1 calc R . . . .
C48 C 0.7523(2) 0.6792(2) 0.73461(15) 0.0295(5) Uani 1 1 d . . . . .
H48a H 0.691288 0.726611 0.742646 0.035 Uiso 1 1 calc R . . . .
H48b H 0.754235 0.653187 0.675975 0.035 Uiso 1 1 calc R . . . .
C49 C 0.5574(2) 0.9279(2) 0.76048(15) 0.0324(6) Uani 1 1 d . . . . .
H49a H 0.509653 0.854205 0.773302 0.039 Uiso 1 1 calc R . . . .
H49b H 0.504888 0.983154 0.754983 0.039 Uiso 1 1 calc R . . . .
C50 C 0.6596(2) 0.9846(2) 0.82528(14) 0.0296(5) Uani 1 1 d . . . . .
H50a H 0.696155 0.924296 0.844803 0.036 Uiso 1 1 calc R . . . .
H50b H 0.634240 1.034110 0.871445 0.036 Uiso 1 1 calc R . . . .
C51 C 0.7433(3) 1.0596(3) 0.77974(17) 0.0521(8) Uani 1 1 d . . . . .
H51a H 0.827432 1.068011 0.800770 0.063 Uiso 1 1 calc R . . . .
H51b H 0.726923 1.139720 0.783852 0.063 Uiso 1 1 calc R . . . .
C52 C 0.7173(3) 0.9909(2) 0.69277(15) 0.0373(6) Uani 1 1 d . . . . .
H52a H 0.706804 1.044940 0.655528 0.045 Uiso 1 1 calc R . . . .
H52b H 0.784081 0.953895 0.677686 0.045 Uiso 1 1 calc R . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Cl1 2.274(9) . ?
Ni1 O1 1.873(3) . ?
Ni1 N1 1.8975(15) . ?
Ni1 N2 1.8467(15) . ?
Ni1 N3 1.9027(15) . ?
P1 N1 1.6140(16) . ?
P1 C13 1.8104(19) . ?
P1 C19 1.8005(19) . ?
P1 C25 1.7934(19) . ?
P2 N3 1.6086(16) . ?
P2 C26 1.8076(19) . ?
P2 C32 1.7972(19) . ?
P2 C38 1.7935(19) . ?
O1 C39 1.347(3) . ?
O2 C45 1.423(3) . ?
O2 C48 1.434(3) . ?
O3 C49 1.423(3) . ?
O3 C52 1.421(3) . ?
N1 C1 1.416(2) . ?
N2 C6 1.391(2) . ?
N2 C7 1.383(2) . ?
N3 C12 1.417(2) . ?
C1 C2 1.391(3) . ?
C1 C6 1.426(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.406(3) . ?
C7 C8 1.406(3) . ?
C7 C12 1.428(3) . ?
C8 C9 1.394(3) . ?
C9 C10 1.380(3) . ?
C10 C11 1.397(3) . ?
C11 C12 1.391(3) . ?
C13 C14 1.400(3) . ?
C13 C18 1.389(3) . ?
C14 C15 1.385(3) . ?
C15 C16 1.389(3) . ?
C16 C17 1.384(3) . ?
C17 C18 1.389(3) . ?
C19 C20 1.393(3) . ?
C19 C24 1.392(3) . ?
C20 C21 1.387(3) . ?
C21 C22 1.385(3) . ?
C22 C23 1.385(3) . ?
C23 C24 1.391(3) . ?
C26 C27 1.392(3) . ?
C26 C31 1.396(3) . ?
C27 C28 1.390(3) . ?
C28 C29 1.382(3) . ?
C29 C30 1.388(3) . ?
C30 C31 1.383(3) . ?
C32 C33 1.390(3) . ?
C32 C37 1.394(3) . ?
C33 C34 1.389(3) . ?
C34 C35 1.383(3) . ?
C35 C36 1.384(3) . ?
C36 C37 1.387(3) . ?
C39 C40 1.403(3) . ?
C39 C44 1.394(3) . ?
C40 C41 1.393(3) . ?
C41 C42 1.383(3) . ?
C42 C43 1.380(3) . ?
C43 C44 1.387(3) . ?
C45 C46 1.522(4) . ?
C46 C47 1.519(4) . ?
C47 C48 1.515(3) . ?
C49 C50 1.506(3) . ?
C50 C51 1.513(4) . ?
C51 C52 1.526(4) . ?

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 Ni1 N1 94.94(11) . . ?
O1 Ni1 N3 96.06(11) . . ?
N1 Ni1 Cl1 98.7(3) . . ?
N1 Ni1 N3 167.38(7) . . ?
N2 Ni1 Cl1 162.1(4) . . ?
N2 Ni1 O1 169.10(11) . . ?
N2 Ni1 N1 85.48(7) . . ?
N2 Ni1 N3 84.90(7) . . ?
N3 Ni1 Cl1 92.9(3) . . ?
N1 P1 C13 112.90(8) . . ?
N1 P1 C19 112.75(9) . . ?
N1 P1 C25 111.98(9) . . ?
C19 P1 C13 107.41(8) . . ?
C25 P1 C13 102.99(9) . . ?
C25 P1 C19 108.23(9) . . ?
N3 P2 C26 111.86(8) . . ?
N3 P2 C32 113.41(9) . . ?
N3 P2 C38 111.73(9) . . ?
C32 P2 C26 108.51(9) . . ?
C38 P2 C26 103.14(9) . . ?
C38 P2 C32 107.59(9) . . ?
C39 O1 Ni1 115.3(2) . . ?
C45 O2 C48 109.31(18) . . ?
C52 O3 C49 107.93(18) . . ?
P1 N1 Ni1 117.36(9) . . ?
C1 N1 Ni1 112.02(12) . . ?
C1 N1 P1 127.56(13) . . ?
C6 N2 Ni1 115.20(12) . . ?
C7 N2 Ni1 113.91(12) . . ?
C7 N2 C6 128.78(16) . . ?
P2 N3 Ni1 124.06(9) . . ?
C12 N3 Ni1 110.65(12) . . ?
C12 N3 P2 125.24(13) . . ?
N1 C1 C6 113.65(16) . . ?
C2 C1 N1 125.97(17) . . ?
C2 C1 C6 120.22(17) . . ?
C1 C2 C3 120.57(18) . . ?
C4 C3 C2 119.56(18) . . ?
C3 C4 C5 120.66(18) . . ?
C4 C5 C6 120.86(18) . . ?
N2 C6 C1 113.10(16) . . ?
N2 C6 C5 129.26(17) . . ?
C5 C6 C1 117.64(17) . . ?
N2 C7 C8 129.28(17) . . ?
N2 C7 C12 113.02(16) . . ?
C8 C7 C12 117.60(17) . . ?
C9 C8 C7 120.61(18) . . ?
C10 C9 C8 121.35(17) . . ?
C9 C10 C11 119.22(17) . . ?
C12 C11 C10 120.61(17) . . ?
N3 C12 C7 113.35(16) . . ?
C11 C12 N3 126.05(17) . . ?
C11 C12 C7 120.55(17) . . ?
C14 C13 P1 118.53(14) . . ?
C18 C13 P1 121.55(14) . . ?
C18 C13 C14 119.79(17) . . ?
C15 C14 C13 119.81(18) . . ?
C14 C15 C16 120.09(19) . . ?
C17 C16 C15 120.18(19) . . ?
C16 C17 C18 120.15(19) . . ?
C17 C18 C13 119.97(18) . . ?
C20 C19 P1 117.91(14) . . ?
C24 C19 P1 122.34(15) . . ?
C24 C19 C20 119.75(17) . . ?
C21 C20 C19 119.94(18) . . ?
C22 C21 C20 120.25(19) . . ?
C21 C22 C23 120.03(19) . . ?
C22 C23 C24 120.10(19) . . ?
C23 C24 C19 119.92(18) . . ?
C27 C26 P2 122.93(15) . . ?
C27 C26 C31 119.56(18) . . ?
C31 C26 P2 117.38(14) . . ?
C28 C27 C26 119.66(19) . . ?
C29 C28 C27 120.43(19) . . ?
C28 C29 C30 120.13(19) . . ?
C31 C30 C29 119.77(19) . . ?
C30 C31 C26 120.42(19) . . ?
C33 C32 P2 118.48(15) . . ?
C33 C32 C37 120.02(18) . . ?
C37 C32 P2 121.38(15) . . ?
C34 C33 C32 119.9(2) . . ?
C35 C34 C33 119.9(2) . . ?
C34 C35 C36 120.5(2) . . ?
C35 C36 C37 120.0(2) . . ?
C36 C37 C32 119.7(2) . . ?
O1 C39 C40 119.6(2) . . ?
O1 C39 C44 122.8(2) . . ?
C44 C39 C40 117.6(2) . . ?
C41 C40 C39 120.6(2) . . ?
C42 C41 C40 120.9(2) . . ?
C43 C42 C41 118.9(2) . . ?
C42 C43 C44 120.7(2) . . ?
C43 C44 C39 121.3(2) . . ?
O2 C45 C46 107.2(2) . . ?
C47 C46 C45 102.4(2) . . ?
C48 C47 C46 101.8(2) . . ?
O2 C48 C47 106.43(19) . . ?
O3 C49 C50 105.5(2) . . ?
C49 C50 C51 100.9(2) . . ?
C50 C51 C52 104.1(2) . . ?
O3 C52 C51 107.0(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_3694

# Crystallographer: Michael R. Gau

# Compound 4

_database_code_depnum_ccdc_archive 'CCDC 1970112'
loop_
_audit_author_name
_audit_author_address
'Patrick Carroll'
;University of Pennsylvania
United States of America
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;

_audit_creation_date             2019-10-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C42 H40 N3 Na Ni O P2'
_chemical_formula_sum            'C42 H40 N3 Na Ni O P2'
_chemical_formula_weight         746.41

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7438(3)
_cell_length_b                   12.7981(4)
_cell_length_c                   14.4155(5)
_cell_angle_alpha                69.6770(10)
_cell_angle_beta                 83.8800(10)
_cell_angle_gamma                74.4970(10)
_cell_volume                     1790.91(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.552
_cell_measurement_theta_min      2.663
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48983
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         2.664
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                6492
_reflns_number_total             8248
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2018.7-2'
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'Mercury 4.2.0 (Macrae et al., 2008)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+2.4151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0815
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.66600(3) 0.47204(2) 0.70429(2) 0.00714(7) Uani 1 1 d . . . . .
P1 P 0.74963(5) 0.31622(5) 0.62025(4) 0.00870(12) Uani 1 1 d . . . . .
P2 P 0.43855(5) 0.63480(5) 0.76668(4) 0.00718(11) Uani 1 1 d . . . . .
Na1 Na 0.56369(8) 0.39351(7) 0.95610(7) 0.01284(19) Uani 1 1 d . . . . .
O1 O 0.58229(16) 0.21797(14) 0.94623(13) 0.0191(4) Uani 1 1 d . . . . .
N1 N 0.77534(18) 0.32486(16) 0.72407(14) 0.0116(4) Uani 1 1 d . . . . .
N2 N 0.73272(17) 0.45528(15) 0.83007(13) 0.0080(4) Uani 1 1 d . . . . .
N3 N 0.50008(17) 0.60149(15) 0.87349(13) 0.0090(4) Uani 1 1 d . . . . .
C1 C 0.8546(2) 0.28089(18) 0.80521(16) 0.0082(4) Uani 1 1 d . . . . .
C2 C 0.9470(2) 0.17655(18) 0.83226(17) 0.0106(4) Uani 1 1 d . . . . .
H2 H 0.960951 0.128252 0.792898 0.013 Uiso 1 1 calc R . . . .
C3 C 1.0194(2) 0.14280(19) 0.91736(17) 0.0121(5) Uani 1 1 d . . . . .
H3 H 1.082766 0.071630 0.935935 0.015 Uiso 1 1 calc R . . . .
C4 C 0.9985(2) 0.21355(18) 0.97455(16) 0.0110(4) Uani 1 1 d . . . . .
H4 H 1.047095 0.190121 1.032796 0.013 Uiso 1 1 calc R . . . .
C5 C 0.9065(2) 0.31904(18) 0.94741(16) 0.0099(4) Uani 1 1 d . . . . .
H5 H 0.893802 0.366638 0.987308 0.012 Uiso 1 1 calc R . . . .
C6 C 0.83290(19) 0.35560(17) 0.86223(16) 0.0072(4) Uani 1 1 d . . . . .
C7 C 0.7380(2) 0.55437(17) 0.84966(15) 0.0078(4) Uani 1 1 d . . . . .
C8 C 0.8548(2) 0.58532(19) 0.84606(16) 0.0110(4) Uani 1 1 d . . . . .
H8 H 0.933464 0.534385 0.836369 0.013 Uiso 1 1 calc R . . . .
C9 C 0.8583(2) 0.68808(19) 0.85627(17) 0.0129(5) Uani 1 1 d . . . . .
H9 H 0.938641 0.706784 0.853861 0.016 Uiso 1 1 calc R . . . .
C10 C 0.7441(2) 0.76394(19) 0.87005(17) 0.0140(5) Uani 1 1 d . . . . .
H10 H 0.745736 0.834933 0.876524 0.017 Uiso 1 1 calc R . . . .
C11 C 0.6279(2) 0.73484(19) 0.87423(16) 0.0118(4) Uani 1 1 d . . . . .
H11 H 0.550004 0.786964 0.883496 0.014 Uiso 1 1 calc R . . . .
C12 C 0.6218(2) 0.63117(18) 0.86524(15) 0.0075(4) Uani 1 1 d . . . . .
C13 C 0.8930(2) 0.30094(18) 0.54349(16) 0.0105(4) Uani 1 1 d . . . . .
C14 C 0.8990(2) 0.2592(2) 0.46516(18) 0.0168(5) Uani 1 1 d . . . . .
H14 H 0.830375 0.230060 0.456002 0.020 Uiso 1 1 calc R . . . .
C15 C 1.0046(2) 0.2600(2) 0.40057(19) 0.0225(6) Uani 1 1 d . . . . .
H15 H 1.007769 0.231800 0.347255 0.027 Uiso 1 1 calc R . . . .
C16 C 1.1047(2) 0.3017(2) 0.4138(2) 0.0253(6) Uani 1 1 d . . . . .
H16 H 1.176411 0.303161 0.369133 0.030 Uiso 1 1 calc R . . . .
C17 C 1.1008(2) 0.3414(2) 0.4920(2) 0.0263(6) Uani 1 1 d . . . . .
H17 H 1.170810 0.368595 0.501688 0.032 Uiso 1 1 calc R . . . .
C18 C 0.9952(2) 0.3420(2) 0.55675(18) 0.0180(5) Uani 1 1 d . . . . .
H18 H 0.992740 0.370245 0.609923 0.022 Uiso 1 1 calc R . . . .
C19 C 0.6829(2) 0.19773(19) 0.62620(16) 0.0114(4) Uani 1 1 d . . . . .
C20 C 0.5518(2) 0.2152(2) 0.61041(18) 0.0176(5) Uani 1 1 d . . . . .
H20 H 0.496431 0.290368 0.595334 0.021 Uiso 1 1 calc R . . . .
C21 C 0.5019(3) 0.1236(2) 0.61662(19) 0.0245(6) Uani 1 1 d . . . . .
H21 H 0.412706 0.136271 0.605397 0.029 Uiso 1 1 calc R . . . .
C22 C 0.5814(3) 0.0140(2) 0.63902(19) 0.0254(6) Uani 1 1 d . . . . .
H22 H 0.546730 -0.048546 0.643467 0.030 Uiso 1 1 calc R . . . .
C23 C 0.7118(3) -0.0050(2) 0.65506(18) 0.0213(5) Uani 1 1 d . . . . .
H23 H 0.766388 -0.080434 0.670393 0.026 Uiso 1 1 calc R . . . .
C24 C 0.7623(2) 0.08640(19) 0.64870(17) 0.0148(5) Uani 1 1 d . . . . .
H24 H 0.851677 0.073137 0.659730 0.018 Uiso 1 1 calc R . . . .
C25 C 0.6395(2) 0.45077(19) 0.57786(17) 0.0121(5) Uani 1 1 d . . . . .
H25a H 0.550723 0.446828 0.569700 0.014 Uiso 1 1 calc R . . . .
H25b H 0.669405 0.505850 0.518241 0.014 Uiso 1 1 calc R . . . .
C26 C 0.3261(2) 0.77777(18) 0.73114(16) 0.0091(4) Uani 1 1 d . . . . .
C27 C 0.3284(2) 0.85750(19) 0.63673(17) 0.0120(5) Uani 1 1 d . . . . .
H27 H 0.388478 0.837397 0.588647 0.014 Uiso 1 1 calc R . . . .
C28 C 0.2441(2) 0.9661(2) 0.61177(18) 0.0162(5) Uani 1 1 d . . . . .
H28 H 0.247108 1.019826 0.547106 0.019 Uiso 1 1 calc R . . . .
C29 C 0.1560(2) 0.9961(2) 0.68101(18) 0.0184(5) Uani 1 1 d . . . . .
H29 H 0.098912 1.070591 0.664316 0.022 Uiso 1 1 calc R . . . .
C30 C 0.1513(2) 0.9167(2) 0.77528(19) 0.0231(6) Uani 1 1 d . . . . .
H30 H 0.089999 0.936558 0.822761 0.028 Uiso 1 1 calc R . . . .
C31 C 0.2359(2) 0.8088(2) 0.80001(18) 0.0181(5) Uani 1 1 d . . . . .
H31 H 0.232443 0.755228 0.864665 0.022 Uiso 1 1 calc R . . . .
C32 C 0.3357(2) 0.54015(18) 0.77754(16) 0.0093(4) Uani 1 1 d . . . . .
C33 C 0.2763(2) 0.4920(2) 0.86790(17) 0.0136(5) Uani 1 1 d . . . . .
H33 H 0.290429 0.508649 0.924622 0.016 Uiso 1 1 calc R . . . .
C34 C 0.1970(2) 0.4202(2) 0.87503(18) 0.0163(5) Uani 1 1 d . . . . .
H34 H 0.157561 0.387491 0.936785 0.020 Uiso 1 1 calc R . . . .
C35 C 0.1745(2) 0.3955(2) 0.79279(18) 0.0162(5) Uani 1 1 d . . . . .
H35 H 0.120262 0.345995 0.798004 0.019 Uiso 1 1 calc R . . . .
C36 C 0.2321(2) 0.4439(2) 0.70303(19) 0.0192(5) Uani 1 1 d . . . . .
H36 H 0.216799 0.427692 0.646323 0.023 Uiso 1 1 calc R . . . .
C37 C 0.3117(2) 0.5157(2) 0.69530(18) 0.0153(5) Uani 1 1 d . . . . .
H37 H 0.350393 0.548561 0.633244 0.018 Uiso 1 1 calc R . . . .
C38 C 0.5530(2) 0.62669(18) 0.67083(15) 0.0087(4) Uani 1 1 d . . . . .
H38a H 0.605010 0.683051 0.660999 0.010 Uiso 1 1 calc R . . . .
H38b H 0.508113 0.645794 0.608358 0.010 Uiso 1 1 calc R . . . .
C39 C 0.6786(2) 0.11571(19) 0.99367(18) 0.0155(5) Uani 1 1 d . . . . .
H39a H 0.651575 0.078239 1.062457 0.019 Uiso 1 1 calc R . . . .
H39b H 0.761999 0.134179 0.995082 0.019 Uiso 1 1 calc R . . . .
C40 C 0.6912(2) 0.0373(2) 0.9326(2) 0.0216(6) Uani 1 1 d . . . . .
H40a H 0.763795 0.045323 0.884323 0.026 Uiso 1 1 calc R . . . .
H40b H 0.705363 -0.044077 0.975591 0.026 Uiso 1 1 calc R . . . .
C41 C 0.5628(2) 0.0783(2) 0.87989(19) 0.0199(5) Uani 1 1 d . . . . .
H41a H 0.574785 0.072410 0.812668 0.024 Uiso 1 1 calc R . . . .
H41b H 0.501359 0.032772 0.917703 0.024 Uiso 1 1 calc R . . . .
C42 C 0.5155(3) 0.2017(3) 0.8753(3) 0.0419(9) Uani 1 1 d . . . . .
H42a H 0.531668 0.253386 0.808345 0.050 Uiso 1 1 calc R . . . .
H42b H 0.421437 0.219886 0.889345 0.050 Uiso 1 1 calc R . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P1 2.5962(6) . ?
Ni1 Na1 3.5497(9) . ?
Ni1 N1 1.8774(18) . ?
Ni1 N2 1.9422(18) . ?
Ni1 C25 1.993(2) . ?
Ni1 C38 1.950(2) . ?
P1 N1 1.5962(19) . ?
P1 C13 1.806(2) . ?
P1 C19 1.816(2) . ?
P1 C25 1.753(2) . ?
P2 Na1 3.3920(10) . ?
P2 N3 1.6125(18) . ?
P2 C26 1.836(2) . ?
P2 C32 1.805(2) . ?
P2 C38 1.761(2) . ?
Na1 Na1 3.3072(17) 2_667 ?
Na1 O1 2.2546(18) . ?
Na1 N2 2.508(2) . ?
Na1 N3 2.497(2) 2_667 ?
Na1 N3 2.443(2) . ?
Na1 C6 3.050(2) . ?
Na1 C7 3.058(2) . ?
Na1 C12 3.063(2) 2_667 ?
Na1 C12 3.071(2) . ?
O1 C39 1.434(3) . ?
O1 C42 1.410(3) . ?
N1 C1 1.382(3) . ?
N2 C6 1.401(3) . ?
N2 C7 1.408(3) . ?
N3 C12 1.438(3) . ?
C1 C2 1.391(3) . ?
C1 C6 1.425(3) . ?
C2 C3 1.397(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.398(3) . ?
C5 C6 1.401(3) . ?
C7 C8 1.404(3) . ?
C7 C12 1.419(3) . ?
C8 C9 1.384(3) . ?
C9 C10 1.390(3) . ?
C10 C11 1.385(3) . ?
C11 C12 1.396(3) . ?
C13 C14 1.396(3) . ?
C13 C18 1.393(3) . ?
C14 C15 1.388(3) . ?
C15 C16 1.379(4) . ?
C16 C17 1.381(4) . ?
C17 C18 1.390(3) . ?
C19 C20 1.396(3) . ?
C19 C24 1.397(3) . ?
C20 C21 1.387(3) . ?
C21 C22 1.380(4) . ?
C22 C23 1.386(4) . ?
C23 C24 1.388(3) . ?
C26 C27 1.391(3) . ?
C26 C31 1.395(3) . ?
C27 C28 1.390(3) . ?
C28 C29 1.382(3) . ?
C29 C30 1.391(3) . ?
C30 C31 1.384(3) . ?
C32 C33 1.400(3) . ?
C32 C37 1.391(3) . ?
C33 C34 1.383(3) . ?
C34 C35 1.387(3) . ?
C35 C36 1.385(3) . ?
C36 C37 1.385(3) . ?
C39 C40 1.522(3) . ?
C40 C41 1.521(3) . ?
C41 C42 1.505(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Ni1 Na1 120.22(2) . . ?
N1 Ni1 P1 37.66(6) . . ?
N1 Ni1 Na1 91.53(6) . . ?
N1 Ni1 N2 84.08(8) . . ?
N1 Ni1 C25 80.08(8) . . ?
N1 Ni1 C38 174.73(9) . . ?
N2 Ni1 P1 121.61(5) . . ?
N2 Ni1 Na1 43.01(5) . . ?
N2 Ni1 C25 163.71(8) . . ?
N2 Ni1 C38 100.80(8) . . ?
C25 Ni1 P1 42.42(6) . . ?
C25 Ni1 Na1 140.71(7) . . ?
C38 Ni1 P1 137.29(6) . . ?
C38 Ni1 Na1 93.40(6) . . ?
C38 Ni1 C25 94.92(9) . . ?
N1 P1 Ni1 45.94(6) . . ?
N1 P1 C13 113.55(10) . . ?
N1 P1 C19 115.92(10) . . ?
N1 P1 C25 96.03(10) . . ?
C13 P1 Ni1 126.51(7) . . ?
C13 P1 C19 104.38(10) . . ?
C19 P1 Ni1 129.09(7) . . ?
C25 P1 Ni1 50.09(7) . . ?
C25 P1 C13 114.12(11) . . ?
C25 P1 C19 113.25(11) . . ?
N3 P2 Na1 41.94(7) . . ?
N3 P2 C26 111.54(10) . . ?
N3 P2 C32 108.06(10) . . ?
N3 P2 C38 114.45(10) . . ?
C26 P2 Na1 145.96(7) . . ?
C32 P2 Na1 75.40(7) . . ?
C32 P2 C26 103.18(10) . . ?
C38 P2 Na1 102.65(7) . . ?
C38 P2 C26 109.55(10) . . ?
C38 P2 C32 109.44(10) . . ?
P2 Na1 Ni1 51.852(16) . . ?
Na1 Na1 Ni1 116.53(4) 2_667 . ?
Na1 Na1 P2 70.84(3) 2_667 . ?
O1 Na1 Ni1 85.99(5) . . ?
O1 Na1 P2 120.71(5) . . ?
O1 Na1 Na1 153.69(7) . 2_667 ?
O1 Na1 N2 99.07(7) . . ?
O1 Na1 N3 146.85(7) . . ?
O1 Na1 N3 111.60(7) . 2_667 ?
O1 Na1 C6 80.76(6) . . ?
O1 Na1 C7 125.59(7) . . ?
O1 Na1 C12 148.46(7) . . ?
O1 Na1 C12 96.52(7) . 2_667 ?
N2 Na1 Ni1 31.89(4) . . ?
N2 Na1 P2 67.84(4) . . ?
N2 Na1 Na1 107.24(6) . 2_667 ?
N2 Na1 C6 27.01(5) . . ?
N2 Na1 C7 27.06(6) . . ?
N2 Na1 C12 162.62(7) . 2_667 ?
N2 Na1 C12 50.75(6) . . ?
N3 Na1 Ni1 68.36(5) . . ?
N3 Na1 Ni1 162.24(5) 2_667 . ?
N3 Na1 P2 26.18(4) . . ?
N3 Na1 P2 116.32(5) 2_667 . ?
N3 Na1 Na1 47.29(5) 2_667 2_667 ?
N3 Na1 Na1 48.67(5) . 2_667 ?
N3 Na1 N2 70.26(6) . . ?
N3 Na1 N2 136.31(7) 2_667 . ?
N3 Na1 N3 95.96(6) . 2_667 ?
N3 Na1 C6 96.39(6) . . ?
N3 Na1 C6 128.93(7) 2_667 . ?
N3 Na1 C7 112.65(6) 2_667 . ?
N3 Na1 C7 52.13(6) . . ?
N3 Na1 C12 98.79(6) 2_667 . ?
N3 Na1 C12 100.23(6) . 2_667 ?
N3 Na1 C12 27.33(6) . . ?
N3 Na1 C12 27.66(6) 2_667 2_667 ?
C6 Na1 Ni1 49.03(4) . . ?
C6 Na1 P2 94.27(5) . . ?
C6 Na1 Na1 123.83(6) . 2_667 ?
C6 Na1 C7 46.76(6) . . ?
C6 Na1 C12 152.48(6) . 2_667 ?
C6 Na1 C12 73.44(6) . . ?
C7 Na1 Ni1 51.43(4) . . ?
C7 Na1 P2 61.74(4) . . ?
C7 Na1 Na1 80.63(5) . 2_667 ?
C7 Na1 C12 136.00(6) . 2_667 ?
C7 Na1 C12 26.77(5) . . ?
C12 Na1 Ni1 158.49(5) 2_667 . ?
C12 Na1 Ni1 63.45(4) . . ?
C12 Na1 P2 110.20(5) 2_667 . ?
C12 Na1 P2 45.74(4) . . ?
C12 Na1 Na1 57.49(5) 2_667 2_667 ?
C12 Na1 Na1 57.26(5) . 2_667 ?
C12 Na1 C12 114.74(5) 2_667 . ?
C39 O1 Na1 125.74(14) . . ?
C42 O1 Na1 122.02(16) . . ?
C42 O1 C39 111.05(18) . . ?
P1 N1 Ni1 96.39(9) . . ?
C1 N1 Ni1 116.06(14) . . ?
C1 N1 P1 146.08(16) . . ?
Ni1 N2 Na1 105.10(8) . . ?
C6 N2 Ni1 111.23(13) . . ?
C6 N2 Na1 98.60(12) . . ?
C6 N2 C7 119.33(17) . . ?
C7 N2 Ni1 119.13(14) . . ?
C7 N2 Na1 98.82(13) . . ?
P2 N3 Na1 111.88(9) . . ?
P2 N3 Na1 140.86(10) . 2_667 ?
Na1 N3 Na1 84.04(6) . 2_667 ?
C12 N3 P2 111.88(14) . . ?
C12 N3 Na1 101.42(12) . . ?
C12 N3 Na1 98.62(12) . 2_667 ?
N1 C1 C2 126.4(2) . . ?
N1 C1 C6 112.43(18) . . ?
C2 C1 C6 121.16(19) . . ?
C1 C2 C3 120.0(2) . . ?
C4 C3 C2 119.7(2) . . ?
C3 C4 C5 120.7(2) . . ?
C4 C5 C6 121.0(2) . . ?
N2 C6 Na1 54.39(10) . . ?
N2 C6 C1 115.60(18) . . ?
N2 C6 C5 126.73(19) . . ?
C1 C6 Na1 114.20(13) . . ?
C5 C6 Na1 98.98(13) . . ?
C5 C6 C1 117.51(19) . . ?
N2 C7 Na1 54.13(10) . . ?
N2 C7 C12 119.69(19) . . ?
C8 C7 Na1 148.72(15) . . ?
C8 C7 N2 121.88(19) . . ?
C8 C7 C12 118.21(19) . . ?
C12 C7 Na1 77.10(12) . . ?
C9 C8 C7 121.7(2) . . ?
C8 C9 C10 120.0(2) . . ?
C11 C10 C9 119.2(2) . . ?
C10 C11 C12 122.0(2) . . ?
Na1 C12 Na1 65.26(5) 2_667 . ?
N3 C12 Na1 51.25(10) . . ?
N3 C12 Na1 53.71(10) . 2_667 ?
C7 C12 Na1 130.15(14) . 2_667 ?
C7 C12 Na1 76.13(12) . . ?
C7 C12 N3 120.42(18) . . ?
C11 C12 Na1 150.03(15) . . ?
C11 C12 Na1 86.85(13) . 2_667 ?
C11 C12 N3 120.67(19) . . ?
C11 C12 C7 118.91(19) . . ?
C14 C13 P1 121.51(17) . . ?
C18 C13 P1 119.10(17) . . ?
C18 C13 C14 119.1(2) . . ?
C15 C14 C13 120.5(2) . . ?
C16 C15 C14 120.0(2) . . ?
C15 C16 C17 120.0(2) . . ?
C16 C17 C18 120.6(2) . . ?
C17 C18 C13 119.9(2) . . ?
C20 C19 P1 121.09(18) . . ?
C20 C19 C24 118.8(2) . . ?
C24 C19 P1 120.13(17) . . ?
C21 C20 C19 120.4(2) . . ?
C22 C21 C20 120.2(2) . . ?
C21 C22 C23 120.1(2) . . ?
C22 C23 C24 119.9(2) . . ?
C23 C24 C19 120.5(2) . . ?
P1 C25 Ni1 87.49(9) . . ?
C27 C26 P2 121.76(17) . . ?
C27 C26 C31 118.5(2) . . ?
C31 C26 P2 119.79(17) . . ?
C28 C27 C26 120.9(2) . . ?
C29 C28 C27 120.0(2) . . ?
C28 C29 C30 119.7(2) . . ?
C31 C30 C29 120.1(2) . . ?
C30 C31 C26 120.8(2) . . ?
C33 C32 P2 120.95(17) . . ?
C37 C32 P2 120.39(17) . . ?
C37 C32 C33 118.6(2) . . ?
C34 C33 C32 120.3(2) . . ?
C33 C34 C35 120.6(2) . . ?
C36 C35 C34 119.3(2) . . ?
C35 C36 C37 120.5(2) . . ?
C36 C37 C32 120.6(2) . . ?
P2 C38 Ni1 109.83(11) . . ?
O1 C39 C40 105.97(19) . . ?
C41 C40 C39 104.20(19) . . ?
C42 C41 C40 103.8(2) . . ?
O1 C42 C41 108.3(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_3376

# Crystallographer: Michael R. Gau

# Compound 5

_database_code_depnum_ccdc_archive 'CCDC 1970110'
loop_
_audit_author_name
_audit_author_address
'Patrick Carroll'
;University of Pennsylvania
United States of America
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;

_audit_creation_date             2018-04-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_formula_moiety         'C38 H33 N3 Ni P2, C7 H8'
_chemical_formula_sum            'C45 H41 N3 Ni P2'
_chemical_formula_weight         744.46

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0629(4)
_cell_length_b                   12.4737(5)
_cell_length_c                   15.2136(6)
_cell_angle_alpha                74.272(2)
_cell_angle_beta                 87.324(2)
_cell_angle_gamma                79.697(2)
_cell_volume                     1808.50(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.514
_cell_measurement_theta_min      2.902
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.857
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016/2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            76559
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         2.903
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                6868
_reflns_number_total             8318
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2016.1-0'
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'Mercury 4.2.0 (Macrae et al., 2008)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+2.1304P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0880
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.53018(2) 0.83112(2) 0.44594(2) 0.00922(7) Uani 1 1 d . . . . .
P1 P 0.68418(5) 0.78093(4) 0.62120(3) 0.00909(11) Uani 1 1 d . . . . .
P2 P 0.63556(5) 0.78784(4) 0.29874(3) 0.00987(11) Uani 1 1 d . . . . .
N1 N 0.54339(16) 0.83898(14) 0.56967(11) 0.0113(3) Uani 1 1 d . . . . .
N2 N 0.34455(16) 0.85127(14) 0.46519(11) 0.0101(3) Uani 1 1 d . . . . .
N3 N 0.48604(16) 0.83333(15) 0.32883(11) 0.0125(3) Uani 1 1 d . . . . .
C1 C 0.41304(19) 0.85765(16) 0.60909(14) 0.0095(4) Uani 1 1 d . . . . .
C2 C 0.3857(2) 0.87662(17) 0.69460(14) 0.0124(4) Uani 1 1 d . . . . .
H2 H 0.458136 0.880286 0.730988 0.015 Uiso 1 1 calc R . . . .
C3 C 0.2539(2) 0.89039(17) 0.72796(14) 0.0135(4) Uani 1 1 d . . . . .
H3 H 0.236824 0.902983 0.786614 0.016 Uiso 1 1 calc R . . . .
C4 C 0.1484(2) 0.88551(17) 0.67478(14) 0.0134(4) Uani 1 1 d . . . . .
H4 H 0.059023 0.891199 0.698218 0.016 Uiso 1 1 calc R . . . .
C5 C 0.1726(2) 0.87230(17) 0.58700(14) 0.0128(4) Uani 1 1 d . . . . .
H5 H 0.098794 0.870884 0.550812 0.015 Uiso 1 1 calc R . . . .
C6 C 0.30368(19) 0.86106(16) 0.55114(13) 0.0094(4) Uani 1 1 d . . . . .
C7 C 0.26771(19) 0.85709(16) 0.39008(14) 0.0104(4) Uani 1 1 d . . . . .
C8 C 0.1272(2) 0.88056(16) 0.37647(14) 0.0120(4) Uani 1 1 d . . . . .
H8 H 0.069122 0.898592 0.423399 0.014 Uiso 1 1 calc R . . . .
C9 C 0.0716(2) 0.87773(17) 0.29466(14) 0.0136(4) Uani 1 1 d . . . . .
H9 H -0.023750 0.893645 0.287179 0.016 Uiso 1 1 calc R . . . .
C10 C 0.1526(2) 0.85220(18) 0.22431(14) 0.0146(4) Uani 1 1 d . . . . .
H10 H 0.113242 0.847029 0.170360 0.017 Uiso 1 1 calc R . . . .
C11 C 0.2932(2) 0.83415(17) 0.23391(14) 0.0129(4) Uani 1 1 d . . . . .
H11 H 0.349961 0.818267 0.185717 0.015 Uiso 1 1 calc R . . . .
C12 C 0.34937(19) 0.83945(16) 0.31362(14) 0.0105(4) Uani 1 1 d . . . . .
C13 C 0.69060(19) 0.76705(17) 0.74291(14) 0.0125(4) Uani 1 1 d . . . . .
C14 C 0.7324(2) 0.85163(18) 0.77426(15) 0.0173(4) Uani 1 1 d . . . . .
H14 H 0.756046 0.916673 0.731812 0.021 Uiso 1 1 calc R . . . .
C15 C 0.7393(2) 0.8402(2) 0.86707(16) 0.0236(5) Uani 1 1 d . . . . .
H15 H 0.768144 0.897488 0.888039 0.028 Uiso 1 1 calc R . . . .
C16 C 0.7043(2) 0.7460(2) 0.92974(16) 0.0248(5) Uani 1 1 d . . . . .
H16 H 0.708761 0.738952 0.993342 0.030 Uiso 1 1 calc R . . . .
C17 C 0.6628(2) 0.6622(2) 0.89925(16) 0.0232(5) Uani 1 1 d . . . . .
H17 H 0.639111 0.597441 0.942089 0.028 Uiso 1 1 calc R . . . .
C18 C 0.6557(2) 0.67243(19) 0.80618(15) 0.0177(4) Uani 1 1 d . . . . .
H18 H 0.626911 0.614803 0.785656 0.021 Uiso 1 1 calc R . . . .
C19 C 0.7350(2) 0.63822(16) 0.61167(13) 0.0112(4) Uani 1 1 d . . . . .
C20 C 0.6340(2) 0.57610(18) 0.60704(15) 0.0157(4) Uani 1 1 d . . . . .
H20 H 0.541712 0.610616 0.605466 0.019 Uiso 1 1 calc R . . . .
C21 C 0.6685(2) 0.46415(19) 0.60475(15) 0.0209(5) Uani 1 1 d . . . . .
H21 H 0.599814 0.421460 0.603139 0.025 Uiso 1 1 calc R . . . .
C22 C 0.8030(2) 0.41468(19) 0.60482(16) 0.0221(5) Uani 1 1 d . . . . .
H22 H 0.826467 0.338077 0.603000 0.026 Uiso 1 1 calc R . . . .
C23 C 0.9032(2) 0.4760(2) 0.60752(17) 0.0243(5) Uani 1 1 d . . . . .
H23 H 0.995279 0.441825 0.606302 0.029 Uiso 1 1 calc R . . . .
C24 C 0.8701(2) 0.58793(18) 0.61202(16) 0.0189(5) Uani 1 1 d . . . . .
H24 H 0.939301 0.629464 0.615308 0.023 Uiso 1 1 calc R . . . .
C25 C 0.8157(2) 0.85904(17) 0.57441(14) 0.0137(4) Uani 1 1 d . . . . .
H25a H 0.834994 0.853786 0.511827 0.021 Uiso 1 1 calc GR . . . .
H25b H 0.897394 0.827594 0.611808 0.021 Uiso 1 1 calc GR . . . .
H25c H 0.786780 0.938488 0.573976 0.021 Uiso 1 1 calc GR . . . .
C26 C 0.66444(19) 0.64373(17) 0.29072(14) 0.0128(4) Uani 1 1 d . . . . .
C27 C 0.6291(2) 0.61996(19) 0.21120(15) 0.0176(4) Uani 1 1 d . . . . .
H27 H 0.595621 0.680235 0.159967 0.021 Uiso 1 1 calc R . . . .
C28 C 0.6426(2) 0.5088(2) 0.20639(17) 0.0220(5) Uani 1 1 d . . . . .
H28 H 0.617905 0.493227 0.152200 0.026 Uiso 1 1 calc R . . . .
C29 C 0.6923(2) 0.42063(19) 0.28109(16) 0.0207(5) Uani 1 1 d . . . . .
H29 H 0.702946 0.344680 0.277580 0.025 Uiso 1 1 calc R . . . .
C30 C 0.7262(2) 0.44308(19) 0.36051(16) 0.0206(5) Uani 1 1 d . . . . .
H30 H 0.759432 0.382432 0.411569 0.025 Uiso 1 1 calc R . . . .
C31 C 0.7120(2) 0.55420(18) 0.36598(15) 0.0178(4) Uani 1 1 d . . . . .
H31 H 0.734584 0.569177 0.420907 0.021 Uiso 1 1 calc R . . . .
C32 C 0.6776(2) 0.87077(17) 0.18705(14) 0.0121(4) Uani 1 1 d . . . . .
C33 C 0.8057(2) 0.84629(19) 0.15005(14) 0.0160(4) Uani 1 1 d . . . . .
H33 H 0.867320 0.780872 0.180035 0.019 Uiso 1 1 calc R . . . .
C34 C 0.8422(2) 0.9181(2) 0.06923(15) 0.0201(5) Uani 1 1 d . . . . .
H34 H 0.929189 0.901880 0.043993 0.024 Uiso 1 1 calc R . . . .
C35 C 0.7522(2) 1.0133(2) 0.02525(15) 0.0219(5) Uani 1 1 d . . . . .
H35 H 0.778179 1.062668 -0.029609 0.026 Uiso 1 1 calc R . . . .
C36 C 0.6245(2) 1.03681(19) 0.06094(15) 0.0201(5) Uani 1 1 d . . . . .
H36 H 0.562526 1.101490 0.030077 0.024 Uiso 1 1 calc R . . . .
C37 C 0.5872(2) 0.96553(18) 0.14210(15) 0.0154(4) Uani 1 1 d . . . . .
H37 H 0.499727 0.981720 0.166766 0.019 Uiso 1 1 calc R . . . .
C38 C 0.71774(19) 0.80651(17) 0.39144(14) 0.0121(4) Uani 1 1 d . . . . .
H38a H 0.762437 0.873773 0.376537 0.014 Uiso 1 1 calc R . . . .
H38b H 0.778626 0.738112 0.426049 0.014 Uiso 1 1 calc R . . . .
C39 C 0.8978(3) 0.3981(2) 0.9106(2) 0.0403(7) Uani 1 1 d . . . . .
C40 C 0.7739(3) 0.3795(2) 0.8850(2) 0.0404(7) Uani 1 1 d . . . . .
H40 H 0.751643 0.395196 0.822267 0.048 Uiso 1 1 calc R . . . .
C41 C 0.6836(3) 0.3377(2) 0.9524(2) 0.0377(7) Uani 1 1 d . . . . .
H41 H 0.597971 0.327537 0.935456 0.045 Uiso 1 1 calc R . . . .
C42 C 0.7173(3) 0.3111(2) 1.0431(2) 0.0384(7) Uani 1 1 d . . . . .
H42 H 0.655155 0.282213 1.088413 0.046 Uiso 1 1 calc R . . . .
C43 C 0.8386(3) 0.3257(3) 1.0683(2) 0.0395(7) Uani 1 1 d . . . . .
H43 H 0.862070 0.305230 1.131114 0.047 Uiso 1 1 calc R . . . .
C44 C 0.9270(3) 0.3695(3) 1.0041(2) 0.0424(7) Uani 1 1 d . . . . .
H44 H 1.010716 0.380938 1.023074 0.051 Uiso 1 1 calc R . . . .
C45 C 0.9938(4) 0.4522(3) 0.8424(2) 0.0648(11) Uani 1 1 d . . . . .
H45a H 0.997597 0.422155 0.788963 0.097 Uiso 1 1 calc GR . . . .
H45b H 1.083863 0.435705 0.869841 0.097 Uiso 1 1 calc GR . . . .
H45c H 0.962880 0.534160 0.823676 0.097 Uiso 1 1 calc GR . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P2 2.5808(6) . ?
Ni1 N1 1.9233(17) . ?
Ni1 N2 1.8598(16) . ?
Ni1 N3 1.8481(17) . ?
Ni1 C38 2.0320(19) . ?
P1 N1 1.6047(17) . ?
P1 C13 1.816(2) . ?
P1 C19 1.805(2) . ?
P1 C25 1.790(2) . ?
P2 N3 1.6020(17) . ?
P2 C26 1.805(2) . ?
P2 C32 1.809(2) . ?
P2 C38 1.756(2) . ?
N1 C1 1.424(2) . ?
N2 C6 1.383(3) . ?
N2 C7 1.388(3) . ?
N3 C12 1.390(2) . ?
C1 C2 1.391(3) . ?
C1 C6 1.430(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.394(3) . ?
C5 C6 1.402(3) . ?
C7 C8 1.406(3) . ?
C7 C12 1.436(3) . ?
C8 C9 1.400(3) . ?
C9 C10 1.386(3) . ?
C10 C11 1.401(3) . ?
C11 C12 1.384(3) . ?
C13 C14 1.403(3) . ?
C13 C18 1.394(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.387(3) . ?
C16 C17 1.386(4) . ?
C17 C18 1.391(3) . ?
C19 C20 1.398(3) . ?
C19 C24 1.391(3) . ?
C20 C21 1.387(3) . ?
C21 C22 1.384(3) . ?
C22 C23 1.377(3) . ?
C23 C24 1.396(3) . ?
C26 C27 1.396(3) . ?
C26 C31 1.398(3) . ?
C27 C28 1.390(3) . ?
C28 C29 1.389(3) . ?
C29 C30 1.382(3) . ?
C30 C31 1.393(3) . ?
C32 C33 1.398(3) . ?
C32 C37 1.389(3) . ?
C33 C34 1.388(3) . ?
C34 C35 1.385(3) . ?
C35 C36 1.385(3) . ?
C36 C37 1.392(3) . ?
C39 C40 1.399(5) . ?
C39 C44 1.400(4) . ?
C39 C45 1.491(5) . ?
C40 C41 1.394(4) . ?
C41 C42 1.372(4) . ?
C42 C43 1.353(4) . ?
C43 C44 1.359(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 P2 151.88(5) . . ?
N1 Ni1 C38 109.93(8) . . ?
N2 Ni1 P2 121.81(5) . . ?
N2 Ni1 N1 85.60(7) . . ?
N2 Ni1 C38 164.45(8) . . ?
N3 Ni1 P2 38.07(5) . . ?
N3 Ni1 N1 170.05(7) . . ?
N3 Ni1 N2 84.73(7) . . ?
N3 Ni1 C38 79.77(8) . . ?
C38 Ni1 P2 42.71(6) . . ?
N1 P1 C13 117.40(9) . . ?
N1 P1 C19 111.07(9) . . ?
N1 P1 C25 111.12(9) . . ?
C19 P1 C13 104.25(9) . . ?
C25 P1 C13 104.18(10) . . ?
C25 P1 C19 108.17(9) . . ?
N3 P2 Ni1 45.35(6) . . ?
N3 P2 C26 115.10(9) . . ?
N3 P2 C32 111.62(9) . . ?
N3 P2 C38 95.73(9) . . ?
C26 P2 Ni1 118.95(7) . . ?
C26 P2 C32 104.96(9) . . ?
C32 P2 Ni1 135.73(7) . . ?
C38 P2 Ni1 51.72(6) . . ?
C38 P2 C26 113.91(10) . . ?
C38 P2 C32 115.84(9) . . ?
P1 N1 Ni1 116.59(9) . . ?
C1 N1 Ni1 111.03(13) . . ?
C1 N1 P1 127.93(14) . . ?
C6 N2 Ni1 115.36(13) . . ?
C6 N2 C7 129.73(17) . . ?
C7 N2 Ni1 114.88(13) . . ?
P2 N3 Ni1 96.58(9) . . ?
C12 N3 Ni1 115.17(13) . . ?
C12 N3 P2 144.23(15) . . ?
N1 C1 C6 114.48(17) . . ?
C2 C1 N1 125.92(18) . . ?
C2 C1 C6 119.55(17) . . ?
C1 C2 C3 121.23(19) . . ?
C4 C3 C2 119.37(19) . . ?
C3 C4 C5 120.40(18) . . ?
C4 C5 C6 121.23(19) . . ?
N2 C6 C1 113.45(16) . . ?
N2 C6 C5 128.64(18) . . ?
C5 C6 C1 117.91(18) . . ?
N2 C7 C8 131.04(18) . . ?
N2 C7 C12 112.49(17) . . ?
C8 C7 C12 116.43(18) . . ?
C9 C8 C7 120.85(18) . . ?
C10 C9 C8 121.47(19) . . ?
C9 C10 C11 119.05(19) . . ?
C12 C11 C10 119.99(19) . . ?
N3 C12 C7 112.29(17) . . ?
C11 C12 N3 125.76(18) . . ?
C11 C12 C7 121.90(18) . . ?
C14 C13 P1 119.95(16) . . ?
C18 C13 P1 120.80(16) . . ?
C18 C13 C14 119.2(2) . . ?
C15 C14 C13 120.0(2) . . ?
C14 C15 C16 120.6(2) . . ?
C17 C16 C15 119.8(2) . . ?
C16 C17 C18 120.3(2) . . ?
C17 C18 C13 120.2(2) . . ?
C20 C19 P1 118.21(15) . . ?
C24 C19 P1 122.06(16) . . ?
C24 C19 C20 119.69(19) . . ?
C21 C20 C19 120.1(2) . . ?
C22 C21 C20 120.0(2) . . ?
C23 C22 C21 120.3(2) . . ?
C22 C23 C24 120.4(2) . . ?
C19 C24 C23 119.5(2) . . ?
C27 C26 P2 120.01(16) . . ?
C27 C26 C31 119.1(2) . . ?
C31 C26 P2 120.66(17) . . ?
C28 C27 C26 120.5(2) . . ?
C29 C28 C27 119.8(2) . . ?
C30 C29 C28 120.2(2) . . ?
C29 C30 C31 120.3(2) . . ?
C30 C31 C26 120.1(2) . . ?
C33 C32 P2 120.16(16) . . ?
C37 C32 P2 119.65(15) . . ?
C37 C32 C33 119.90(19) . . ?
C34 C33 C32 119.6(2) . . ?
C35 C34 C33 120.3(2) . . ?
C36 C35 C34 120.2(2) . . ?
C35 C36 C37 119.9(2) . . ?
C32 C37 C36 120.0(2) . . ?
P2 C38 Ni1 85.57(8) . . ?
C40 C39 C44 117.6(3) . . ?
C40 C39 C45 122.1(3) . . ?
C44 C39 C45 120.2(3) . . ?
C41 C40 C39 119.4(3) . . ?
C42 C41 C40 120.5(3) . . ?
C43 C42 C41 120.4(3) . . ?
C42 C43 C44 120.3(3) . . ?
C43 C44 C39 121.7(3) . . ?

####################################################################### 
# 
# 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_3593

# Crystallographer: Patrick J. Carroll

# Compound 6

_database_code_depnum_ccdc_archive 'CCDC 1970111'
loop_
_audit_author_name
_audit_author_address
'Patrick Carroll'
;University of Pennsylvania
United States of America
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;

_audit_creation_date             2020-04-21
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r6015)
;
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C47 H42 N4 Ni P2, C2 H3 N'
_chemical_formula_sum            'C49 H45 N5 Ni P2'
_chemical_formula_weight         824.55

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   8.8277(6)
_cell_length_b                   26.5464(18)
_cell_length_c                   17.2437(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.715(3)
_cell_angle_gamma                90
_cell_volume                     4027.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9012
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.95
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.894
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            114083
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         2.824
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_number_gt                7582
_reflns_number_total             9287
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT v8.37A'
_computing_data_collection       'Bruker APEX3 v2016.1-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury 4.2.0 (Macrae et al., 2008)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT v2014/5 (Sheldrick, 2015)'
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0745
_refine_ls_restrained_S_all      1.246
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+22.5293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1691
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.48978(6) 0.28918(2) 0.36332(3) 0.01437(13) Uani 1 1 d . . . . .
P1 P 0.18064(12) 0.23986(4) 0.33769(6) 0.0144(2) Uani 1 1 d . . . . .
P2 P 0.59899(12) 0.38246(4) 0.44151(7) 0.0157(2) Uani 1 1 d . . . . .
N1 N 0.3507(4) 0.24354(14) 0.3081(2) 0.0161(7) Uani 1 1 d . . . . .
N2 N 0.5972(4) 0.23134(13) 0.3957(2) 0.0152(7) Uani 1 1 d . . . . .
N3 N 0.6281(4) 0.32224(14) 0.4334(2) 0.0154(7) Uani 1 1 d . . . . .
N4 N 0.3220(4) 0.35585(14) 0.2582(2) 0.0185(8) Uani 1 1 d . . . . .
H4 H 0.285178 0.328043 0.236245 0.022 Uiso 1 1 calc R . . . .
C1 C 0.4269(5) 0.19605(16) 0.2999(2) 0.0153(8) Uani 1 1 d . . . . .
C2 C 0.3751(5) 0.15813(17) 0.2493(3) 0.0191(9) Uani 1 1 d . . . . .
H2 H 0.282927 0.162661 0.217576 0.023 Uiso 1 1 calc R . . . .
C3 C 0.4568(5) 0.11324(18) 0.2442(3) 0.0224(10) Uani 1 1 d . . . . .
H3 H 0.420986 0.087267 0.209464 0.027 Uiso 1 1 calc R . . . .
C4 C 0.5911(5) 0.10751(18) 0.2908(3) 0.0224(10) Uani 1 1 d . . . . .
H4a H 0.648251 0.077391 0.287366 0.027 Uiso 1 1 calc R . . . .
C5 C 0.6439(5) 0.14484(18) 0.3426(3) 0.0199(9) Uani 1 1 d . . . . .
H5 H 0.736376 0.139899 0.373844 0.024 Uiso 1 1 calc R . . . .
C6 C 0.5624(5) 0.18967(16) 0.3492(3) 0.0159(8) Uani 1 1 d . . . . .
C7 C 0.7081(4) 0.23813(18) 0.4568(2) 0.0168(9) Uani 1 1 d . . . . .
C8 C 0.7975(5) 0.20203(18) 0.4981(3) 0.0192(9) Uani 1 1 d . . . . .
H8 H 0.790035 0.167584 0.483314 0.023 Uiso 1 1 calc R . . . .
C9 C 0.8982(5) 0.2166(2) 0.5614(3) 0.0224(10) Uani 1 1 d . . . . .
H9 H 0.958290 0.191844 0.589326 0.027 Uiso 1 1 calc R . . . .
C10 C 0.9110(5) 0.26642(19) 0.5836(3) 0.0204(9) Uani 1 1 d . . . . .
H10 H 0.979596 0.275864 0.626432 0.025 Uiso 1 1 calc R . . . .
C11 C 0.8227(5) 0.30310(18) 0.5427(3) 0.0192(9) Uani 1 1 d . . . . .
H11 H 0.830996 0.337363 0.558408 0.023 Uiso 1 1 calc R . . . .
C12 C 0.7231(4) 0.28981(18) 0.4795(2) 0.0166(8) Uani 1 1 d . . . . .
C13 C 0.0339(4) 0.24697(17) 0.2596(3) 0.0171(9) Uani 1 1 d . . . . .
C14 C -0.1191(5) 0.25313(18) 0.2758(3) 0.0204(9) Uani 1 1 d . . . . .
H14 H -0.145869 0.252739 0.328048 0.024 Uiso 1 1 calc R . . . .
C15 C -0.2296(5) 0.25975(18) 0.2151(3) 0.0220(10) Uani 1 1 d . . . . .
H15 H -0.332942 0.263532 0.225701 0.026 Uiso 1 1 calc R . . . .
C16 C -0.1907(5) 0.26090(19) 0.1387(3) 0.0217(10) Uani 1 1 d . . . . .
H16 H -0.267303 0.265805 0.097354 0.026 Uiso 1 1 calc R . . . .
C17 C -0.0395(5) 0.25487(19) 0.1224(3) 0.0224(10) Uani 1 1 d . . . . .
H17 H -0.013153 0.255380 0.070093 0.027 Uiso 1 1 calc R . . . .
C18 C 0.0725(5) 0.24811(17) 0.1831(2) 0.0170(9) Uani 1 1 d . . . . .
H18 H 0.175606 0.244273 0.172260 0.020 Uiso 1 1 calc R . . . .
C19 C 0.1519(5) 0.18155(17) 0.3877(3) 0.0169(9) Uani 1 1 d . . . . .
C20 C 0.0436(5) 0.14641(17) 0.3607(3) 0.0191(9) Uani 1 1 d . . . . .
H20 H -0.015760 0.151852 0.312932 0.023 Uiso 1 1 calc R . . . .
C21 C 0.0229(5) 0.10304(18) 0.4042(3) 0.0233(10) Uani 1 1 d . . . . .
H21 H -0.051247 0.078987 0.385875 0.028 Uiso 1 1 calc R . . . .
C22 C 0.1083(5) 0.09459(18) 0.4734(3) 0.0247(10) Uani 1 1 d . . . . .
H22 H 0.092191 0.065175 0.503003 0.030 Uiso 1 1 calc R . . . .
C23 C 0.2186(5) 0.1296(2) 0.4997(3) 0.0255(10) Uani 1 1 d . . . . .
H23 H 0.278001 0.124001 0.547363 0.031 Uiso 1 1 calc R . . . .
C24 C 0.2415(5) 0.17222(18) 0.4565(3) 0.0211(9) Uani 1 1 d . . . . .
H24 H 0.318971 0.195408 0.473840 0.025 Uiso 1 1 calc R . . . .
C25 C 0.1445(5) 0.28763(18) 0.4076(3) 0.0188(9) Uani 1 1 d . . . . .
H25a H 0.219545 0.284943 0.452561 0.028 Uiso 1 1 calc GR . . . .
H25b H 0.042179 0.283056 0.424707 0.028 Uiso 1 1 calc GR . . . .
H25c H 0.151909 0.320947 0.383760 0.028 Uiso 1 1 calc GR . . . .
C26 C 0.5499(5) 0.39903(18) 0.5383(3) 0.0201(9) Uani 1 1 d . . . . .
C27 C 0.6311(5) 0.4341(2) 0.5849(3) 0.0303(12) Uani 1 1 d . . . . .
H27 H 0.716269 0.450523 0.565948 0.036 Uiso 1 1 calc R . . . .
C28 C 0.5890(6) 0.4454(2) 0.6586(3) 0.0350(13) Uani 1 1 d . . . . .
H28 H 0.644871 0.469631 0.689756 0.042 Uiso 1 1 calc R . . . .
C29 C 0.4660(7) 0.4214(2) 0.6868(3) 0.0346(13) Uani 1 1 d . . . . .
H29 H 0.436746 0.429206 0.737267 0.042 Uiso 1 1 calc R . . . .
C30 C 0.3852(8) 0.3858(2) 0.6411(3) 0.0418(14) Uani 1 1 d . . . . .
H30 H 0.301210 0.368954 0.660487 0.050 Uiso 1 1 calc R . . . .
C31 C 0.4272(6) 0.3749(2) 0.5675(3) 0.0308(12) Uani 1 1 d . . . . .
H31 H 0.371315 0.350647 0.536442 0.037 Uiso 1 1 calc R . . . .
C32 C 0.7615(5) 0.42176(18) 0.4253(3) 0.0195(9) Uani 1 1 d . . . . .
C33 C 0.9088(5) 0.4019(2) 0.4307(3) 0.0268(11) Uani 1 1 d . . . . .
H33 H 0.925097 0.367604 0.445011 0.032 Uiso 1 1 calc R . . . .
C34 C 1.0314(6) 0.4322(2) 0.4153(3) 0.0334(12) Uani 1 1 d . . . . .
H34 H 1.131519 0.418720 0.420082 0.040 Uiso 1 1 calc R . . . .
C35 C 1.0083(6) 0.4813(2) 0.3931(3) 0.0318(12) Uani 1 1 d . . . . .
H35 H 1.092009 0.501474 0.381012 0.038 Uiso 1 1 calc R . . . .
C36 C 0.8642(6) 0.5016(2) 0.3882(4) 0.0390(14) Uani 1 1 d . . . . .
H36 H 0.848902 0.535889 0.373860 0.047 Uiso 1 1 calc R . . . .
C37 C 0.7413(6) 0.4718(2) 0.4044(4) 0.0351(13) Uani 1 1 d . . . . .
H37 H 0.642114 0.485993 0.401000 0.042 Uiso 1 1 calc R . . . .
C38 C 0.4540(5) 0.39421(17) 0.3699(3) 0.0183(9) Uani 1 1 d . . . . .
H38 H 0.408737 0.426362 0.360799 0.022 Uiso 1 1 calc R . . . .
C39 C 0.4115(5) 0.35170(17) 0.3275(3) 0.0173(9) Uani 1 1 d . . . . .
C40 C 0.2858(5) 0.40266(17) 0.2202(3) 0.0191(9) Uani 1 1 d . . . . .
C41 C 0.4028(5) 0.43157(18) 0.1921(3) 0.0215(9) Uani 1 1 d . . . . .
C42 C 0.3677(6) 0.47857(18) 0.1598(3) 0.0245(10) Uani 1 1 d . . . . .
H42 H 0.445305 0.498002 0.139143 0.029 Uiso 1 1 calc R . . . .
C43 C 0.2200(6) 0.4975(2) 0.1575(3) 0.0298(11) Uani 1 1 d . . . . .
H43 H 0.198429 0.530525 0.138251 0.036 Uiso 1 1 calc R . . . .
C44 C 0.1060(6) 0.4682(2) 0.1832(3) 0.0290(11) Uani 1 1 d . . . . .
H44 H 0.005390 0.481181 0.180730 0.035 Uiso 1 1 calc R . . . .
C45 C 0.1340(5) 0.41971(18) 0.2129(3) 0.0223(10) Uani 1 1 d . . . . .
C46 C 0.5648(5) 0.41226(19) 0.1950(3) 0.0253(10) Uani 1 1 d . . . . .
H46a H 0.615481 0.418272 0.246874 0.038 Uiso 1 1 calc GR . . . .
H46b H 0.619751 0.429977 0.156039 0.038 Uiso 1 1 calc GR . . . .
H46c H 0.564034 0.376047 0.183893 0.038 Uiso 1 1 calc GR . . . .
C47 C 0.0060(5) 0.3864(2) 0.2333(3) 0.0274(11) Uani 1 1 d . . . . .
H47a H -0.018451 0.362335 0.190970 0.041 Uiso 1 1 calc GR . . . .
H47b H -0.083626 0.407011 0.240924 0.041 Uiso 1 1 calc GR . . . .
H47c H 0.036382 0.367965 0.281342 0.041 Uiso 1 1 calc GR . . . .
N5 N 0.7480(6) 0.01160(19) 0.4304(3) 0.0392(11) Uani 1 1 d . . . . .
C48 C 0.6714(6) 0.0384(2) 0.4607(3) 0.0316(12) Uani 1 1 d . . . . .
C49 C 0.5705(7) 0.0730(2) 0.4980(4) 0.0399(14) Uani 1 1 d . . . . .
H49a H 0.528113 0.097516 0.459603 0.060 Uiso 1 1 calc GR . . . .
H49b H 0.628247 0.090750 0.540593 0.060 Uiso 1 1 calc GR . . . .
H49c H 0.487704 0.053929 0.518611 0.060 Uiso 1 1 calc GR . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.921(4) . ?
Ni1 N2 1.866(4) . ?
Ni1 N3 1.865(4) . ?
Ni1 C39 1.882(4) . ?
P1 N1 1.628(3) . ?
P1 C13 1.800(4) . ?
P1 C19 1.800(4) . ?
P1 C25 1.797(5) . ?
P2 N3 1.627(4) . ?
P2 C26 1.813(5) . ?
P2 C32 1.814(5) . ?
P2 C38 1.732(4) . ?
N1 C1 1.441(5) . ?
N2 C6 1.385(6) . ?
N2 C7 1.390(5) . ?
N3 C12 1.402(5) . ?
N4 C39 1.381(6) . ?
N4 C40 1.429(6) . ?
C1 C2 1.385(6) . ?
C1 C6 1.420(6) . ?
C2 C3 1.399(6) . ?
C3 C4 1.385(6) . ?
C4 C5 1.388(7) . ?
C5 C6 1.400(6) . ?
C7 C8 1.399(6) . ?
C7 C12 1.430(7) . ?
C8 C9 1.405(6) . ?
C9 C10 1.378(7) . ?
C10 C11 1.400(6) . ?
C11 C12 1.388(6) . ?
C13 C14 1.411(6) . ?
C13 C18 1.388(6) . ?
C14 C15 1.383(6) . ?
C15 C16 1.389(7) . ?
C16 C17 1.396(6) . ?
C17 C18 1.391(6) . ?
C19 C20 1.388(6) . ?
C19 C24 1.393(6) . ?
C20 C21 1.395(7) . ?
C21 C22 1.376(7) . ?
C22 C23 1.393(7) . ?
C23 C24 1.379(7) . ?
C26 C27 1.389(7) . ?
C26 C31 1.388(7) . ?
C27 C28 1.387(7) . ?
C28 C29 1.382(8) . ?
C29 C30 1.389(9) . ?
C30 C31 1.382(7) . ?
C32 C33 1.400(6) . ?
C32 C37 1.385(7) . ?
C33 C34 1.392(7) . ?
C34 C35 1.370(8) . ?
C35 C36 1.378(8) . ?
C36 C37 1.389(7) . ?
C38 C39 1.380(6) . ?
C40 C41 1.405(6) . ?
C40 C45 1.410(6) . ?
C41 C42 1.390(7) . ?
C41 C46 1.517(6) . ?
C42 C43 1.395(7) . ?
C43 C44 1.375(8) . ?
C44 C45 1.400(7) . ?
C45 C47 1.500(7) . ?
N5 C48 1.138(7) . ?
C48 C49 1.464(8) . ?

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
N2 Ni1 N1 85.27(16) . . ?
N2 Ni1 C39 170.94(16) . . ?
N3 Ni1 N1 167.31(16) . . ?
N3 Ni1 N2 84.48(16) . . ?
N3 Ni1 C39 90.06(18) . . ?
C39 Ni1 N1 101.01(18) . . ?
N1 P1 C13 112.6(2) . . ?
N1 P1 C19 111.82(19) . . ?
N1 P1 C25 112.8(2) . . ?
C19 P1 C13 109.1(2) . . ?
C25 P1 C13 105.8(2) . . ?
C25 P1 C19 104.2(2) . . ?
N3 P2 C26 111.6(2) . . ?
N3 P2 C32 114.8(2) . . ?
N3 P2 C38 103.2(2) . . ?
C26 P2 C32 104.7(2) . . ?
C38 P2 C26 113.2(2) . . ?
C38 P2 C32 109.5(2) . . ?
P1 N1 Ni1 116.8(2) . . ?
C1 N1 Ni1 108.4(3) . . ?
C1 N1 P1 115.3(3) . . ?
C6 N2 Ni1 113.7(3) . . ?
C6 N2 C7 130.6(4) . . ?
C7 N2 Ni1 115.4(3) . . ?
P2 N3 Ni1 114.73(19) . . ?
C12 N3 Ni1 114.1(3) . . ?
C12 N3 P2 130.2(3) . . ?
C39 N4 C40 123.9(4) . . ?
C2 C1 N1 124.4(4) . . ?
C2 C1 C6 120.6(4) . . ?
C6 C1 N1 115.0(4) . . ?
C1 C2 C3 120.9(4) . . ?
C4 C3 C2 118.5(4) . . ?
C3 C4 C5 121.4(4) . . ?
C4 C5 C6 120.8(4) . . ?
N2 C6 C1 112.7(4) . . ?
N2 C6 C5 129.5(4) . . ?
C5 C6 C1 117.7(4) . . ?
N2 C7 C8 129.1(4) . . ?
N2 C7 C12 112.1(4) . . ?
C8 C7 C12 118.8(4) . . ?
C7 C8 C9 120.1(4) . . ?
C10 C9 C8 120.8(4) . . ?
C9 C10 C11 119.9(4) . . ?
C12 C11 C10 120.6(4) . . ?
N3 C12 C7 113.3(4) . . ?
C11 C12 N3 126.9(4) . . ?
C11 C12 C7 119.8(4) . . ?
C14 C13 P1 120.3(3) . . ?
C18 C13 P1 119.7(3) . . ?
C18 C13 C14 120.0(4) . . ?
C15 C14 C13 119.5(4) . . ?
C14 C15 C16 120.5(4) . . ?
C15 C16 C17 120.2(4) . . ?
C18 C17 C16 119.7(4) . . ?
C13 C18 C17 120.2(4) . . ?
C20 C19 P1 122.5(3) . . ?
C20 C19 C24 119.6(4) . . ?
C24 C19 P1 117.9(3) . . ?
C19 C20 C21 119.4(4) . . ?
C22 C21 C20 121.0(4) . . ?
C21 C22 C23 119.4(4) . . ?
C24 C23 C22 120.1(4) . . ?
C23 C24 C19 120.5(4) . . ?
C27 C26 P2 122.9(4) . . ?
C31 C26 P2 118.3(4) . . ?
C31 C26 C27 118.7(5) . . ?
C28 C27 C26 120.7(5) . . ?
C29 C28 C27 120.1(5) . . ?
C28 C29 C30 119.7(5) . . ?
C31 C30 C29 120.0(5) . . ?
C30 C31 C26 120.9(5) . . ?
C33 C32 P2 121.0(4) . . ?
C37 C32 P2 120.4(4) . . ?
C37 C32 C33 118.6(4) . . ?
C34 C33 C32 120.1(5) . . ?
C35 C34 C33 120.2(5) . . ?
C34 C35 C36 120.4(5) . . ?
C35 C36 C37 119.8(5) . . ?
C32 C37 C36 120.8(5) . . ?
C39 C38 P2 112.5(3) . . ?
N4 C39 Ni1 121.5(3) . . ?
C38 C39 Ni1 118.1(3) . . ?
C38 C39 N4 120.3(4) . . ?
C41 C40 N4 119.4(4) . . ?
C41 C40 C45 120.9(4) . . ?
C45 C40 N4 119.7(4) . . ?
C40 C41 C46 121.5(4) . . ?
C42 C41 C40 118.9(4) . . ?
C42 C41 C46 119.7(4) . . ?
C41 C42 C43 120.8(5) . . ?
C44 C43 C42 119.6(5) . . ?
C43 C44 C45 121.8(5) . . ?
C40 C45 C47 121.2(4) . . ?
C44 C45 C40 117.8(4) . . ?
C44 C45 C47 121.0(4) . . ?
N5 C48 C49 178.6(6) . . ?

