#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/81/4318177.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4318177
loop_
_publ_author_name
'Jitendra K. Bera'
'Paul S. Szalay'
'Kim R. Dunbar'
_publ_section_title
;
 A Study of Structural and Bonding Variations in the Homologous Series
 [Mo2(CN)6(dppm)2]n- (n= 2, 1, 0)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3429
_journal_page_last               3436
_journal_paper_doi               10.1021/ic020157n
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C58 H50 Mo2 N8 O4 P4'
_chemical_formula_weight         1238.82
_chemical_name_systematic
;
di(bis(diphenylphosphino)methane)hexacyanodimolybdate
.2 nitromethane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.47(3)
_cell_angle_beta                 107.12(3)
_cell_angle_gamma                91.86(3)
_cell_formula_units_Z            1
_cell_length_a                   9.942(2)
_cell_length_b                   12.418(3)
_cell_length_c                   12.934(3)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      1.65
_cell_volume                     1516.0(7)
_computing_cell_refinement       'SAINT v4.05 (Siemens, 1996)'
_computing_data_collection       'SMART V4.05 (Siemens, 1996)'
_computing_data_reduction        'XPREP SHELXTL v5 (Siemens, 1994)'
_computing_molecular_graphics    'XP SHELXTL v5 (Siemens, 1994)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '5.7 pixels mm-1'
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type
'Siemens Smart 1K CCD Area Detector Diffractometer'
_diffrn_measurement_method       'Omega Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0650
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18034
_diffrn_reflns_theta_full        28.16
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          1.650
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0758P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                4948
_reflns_number_total             7021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020157n_3.cif
_cod_data_source_block           Mo(III,III)
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        1516.1(5)
_cod_database_code               4318177
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.51986(3) 0.38936(2) 0.53029(2) 0.02021(9) Uani 1 1 d . . .
P1 P 0.68154(8) 0.46548(6) 0.71699(6) 0.02175(18) Uani 1 1 d . . .
P2 P 0.64039(8) 0.69734(6) 0.65388(6) 0.02203(18) Uani 1 1 d . . .
C1 C 0.3992(3) 0.2874(3) 0.6035(3) 0.0256(7) Uani 1 1 d . . .
C2 C 0.6552(3) 0.2464(3) 0.5497(3) 0.0245(7) Uani 1 1 d . . .
C3 C 0.3784(3) 0.4997(3) 0.5605(3) 0.0262(7) Uani 1 1 d . . .
C4 C 0.6421(3) 0.6047(3) 0.7587(2) 0.0256(7) Uani 1 1 d . . .
H4A H 0.7124 0.6327 0.8264 0.031 Uiso 1 1 calc R . .
H4B H 0.5508 0.6027 0.7718 0.031 Uiso 1 1 calc R . .
C11 C 0.6589(4) 0.3887(3) 0.8260(3) 0.0273(7) Uani 1 1 d . . .
C12 C 0.7357(6) 0.2991(4) 0.8500(4) 0.0622(14) Uani 1 1 d . . .
H12A H 0.8020 0.2814 0.8143 0.075 Uiso 1 1 calc R . .
C13 C 0.7147(7) 0.2349(4) 0.9272(4) 0.084(2) Uani 1 1 d . . .
H13A H 0.7674 0.1747 0.9427 0.101 Uiso 1 1 calc R . .
C14 C 0.6175(6) 0.2594(4) 0.9803(4) 0.0592(13) Uani 1 1 d . . .
H14A H 0.6063 0.2177 1.0337 0.071 Uiso 1 1 calc R . .
C15 C 0.5375(5) 0.3450(4) 0.9545(4) 0.0548(12) Uani 1 1 d . . .
H15A H 0.4679 0.3601 0.9877 0.066 Uiso 1 1 calc R . .
C16 C 0.5594(4) 0.4103(4) 0.8785(3) 0.0454(10) Uani 1 1 d . . .
H16A H 0.5056 0.4699 0.8628 0.054 Uiso 1 1 calc R . .
C21 C 0.8738(3) 0.4727(3) 0.7445(3) 0.0289(7) Uani 1 1 d . . .
C22 C 0.9610(4) 0.5227(4) 0.8449(3) 0.0499(11) Uani 1 1 d . . .
H22A H 0.9216 0.5535 0.8967 0.060 Uiso 1 1 calc R . .
C23 C 1.1066(5) 0.5260(5) 0.8662(4) 0.0726(16) Uani 1 1 d . . .
H23A H 1.1648 0.5599 0.9321 0.087 Uiso 1 1 calc R . .
C24 C 1.1646(5) 0.4792(5) 0.7899(5) 0.0741(16) Uani 1 1 d . . .
H24A H 1.2622 0.4811 0.8055 0.089 Uiso 1 1 calc R . .
C25 C 1.0816(4) 0.4297(4) 0.6915(4) 0.0560(12) Uani 1 1 d . . .
H25A H 1.1224 0.3990 0.6406 0.067 Uiso 1 1 calc R . .
C26 C 0.9351(4) 0.4260(3) 0.6685(3) 0.0366(8) Uani 1 1 d . . .
H26A H 0.8781 0.3922 0.6021 0.044 Uiso 1 1 calc R . .
C31 C 0.8282(3) 0.7344(3) 0.6745(3) 0.0291(7) Uani 1 1 d . . .
C32 C 0.9030(4) 0.8101(3) 0.7612(3) 0.0454(10) Uani 1 1 d . . .
H32A H 0.8578 0.8437 0.8079 0.054 Uiso 1 1 calc R . .
C33 C 1.0465(5) 0.8349(4) 0.7769(4) 0.0598(13) Uani 1 1 d . . .
H33A H 1.0963 0.8857 0.8341 0.072 Uiso 1 1 calc R . .
C34 C 1.1153(4) 0.7849(4) 0.7083(4) 0.0577(12) Uani 1 1 d . . .
H34A H 1.2106 0.8021 0.7193 0.069 Uiso 1 1 calc R . .
C35 C 1.0416(4) 0.7095(4) 0.6238(4) 0.0505(11) Uani 1 1 d . . .
H35A H 1.0877 0.6752 0.5781 0.061 Uiso 1 1 calc R . .
C36 C 0.8979(4) 0.6839(3) 0.6060(3) 0.0369(8) Uani 1 1 d . . .
H36A H 0.8489 0.6332 0.5485 0.044 Uiso 1 1 calc R . .
C41 C 0.5787(3) 0.8234(3) 0.7049(3) 0.0259(7) Uani 1 1 d . . .
C42 C 0.5271(4) 0.8346(3) 0.7930(3) 0.0389(9) Uani 1 1 d . . .
H42A H 0.5248 0.7761 0.8324 0.047 Uiso 1 1 calc R . .
C43 C 0.4779(5) 0.9339(3) 0.8237(4) 0.0514(11) Uani 1 1 d . . .
H43A H 0.4429 0.9407 0.8831 0.062 Uiso 1 1 calc R . .
C44 C 0.4814(5) 1.0209(3) 0.7663(3) 0.0454(10) Uani 1 1 d . . .
H44A H 0.4488 1.0865 0.7867 0.054 Uiso 1 1 calc R . .
C45 C 0.5332(5) 1.0108(3) 0.6787(3) 0.0484(11) Uani 1 1 d . . .
H45A H 0.5365 1.0700 0.6404 0.058 Uiso 1 1 calc R . .
C46 C 0.5808(4) 0.9124(3) 0.6468(3) 0.0415(9) Uani 1 1 d . . .
H46A H 0.6140 0.9060 0.5865 0.050 Uiso 1 1 calc R . .
N1 N 0.3310(3) 0.2360(3) 0.6379(3) 0.0425(8) Uani 1 1 d . . .
N2 N 0.7285(4) 0.1825(3) 0.5609(3) 0.0553(10) Uani 1 1 d . . .
N3 N 0.3208(3) 0.5739(3) 0.5721(2) 0.0366(7) Uani 1 1 d . . .
C50 C 0.8818(15) 0.8307(9) 1.1889(9) 0.210(6) Uani 1 1 d . . .
H50A H 0.8861 0.7591 1.2115 0.314 Uiso 1 1 calc R . .
H50B H 0.8144 0.8694 1.2152 0.314 Uiso 1 1 calc R . .
H50C H 0.9730 0.8685 1.2179 0.314 Uiso 1 1 calc R . .
N50 N 0.8398(11) 0.8232(7) 1.0719(6) 0.163(4) Uani 1 1 d . . .
O1 O 0.8163(8) 0.7462(6) 1.0157(5) 0.167(3) Uani 1 1 d . . .
O2 O 0.835(2) 0.9123(9) 1.0480(10) 0.501(15) Uani 1 1 d . . .
C51 C 0.0572(6) 0.0402(5) 0.5250(5) 0.0957(18) Uiso 0.50 1 d P . .
N51 N 0.0572(6) 0.0402(5) 0.5250(5) 0.0957(18) Uiso 0.50 1 d P . .
O3 O 0.1710(7) 0.0137(5) 0.5308(5) 0.0647(17) Uiso 0.50 1 d P . .
O4 O 0.0197(8) 0.1284(6) 0.5771(6) 0.077(2) Uiso 0.50 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
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
C3 Mo1 C1 80.22(12) . . ?
C3 Mo1 C2 159.02(12) . . ?
C1 Mo1 C2 81.08(11) . . ?
C3 Mo1 C3 95.76(12) . 2_666 ?
C1 Mo1 C3 173.25(12) . 2_666 ?
C2 Mo1 C3 103.72(12) . 2_666 ?
C3 Mo1 N3 123.18(12) . 2_666 ?
C1 Mo1 N3 155.49(12) . 2_666 ?
C2 Mo1 N3 76.80(11) . 2_666 ?
C3 Mo1 N3 27.52(11) 2_666 2_666 ?
C3 Mo1 P1 85.53(9) . . ?
C1 Mo1 P1 91.30(9) . . ?
C2 Mo1 P1 85.48(9) . . ?
C3 Mo1 P1 93.80(9) 2_666 . ?
N3 Mo1 P1 97.29(8) 2_666 . ?
C3 Mo1 P2 96.41(9) . 2_666 ?
C1 Mo1 P2 86.65(9) . 2_666 ?
C2 Mo1 P2 91.89(9) . 2_666 ?
C3 Mo1 P2 88.43(9) 2_666 2_666 ?
N3 Mo1 P2 83.69(8) 2_666 2_666 ?
P1 Mo1 P2 176.90(3) . 2_666 ?
C3 Mo1 Mo1 50.73(9) . 2_666 ?
C1 Mo1 Mo1 130.68(8) . 2_666 ?
C2 Mo1 Mo1 148.04(8) . 2_666 ?
C3 Mo1 Mo1 45.03(9) 2_666 2_666 ?
N3 Mo1 Mo1 72.49(8) 2_666 2_666 ?
P1 Mo1 Mo1 89.78(4) . 2_666 ?
P2 Mo1 Mo1 93.33(4) 2_666 2_666 ?
C21 P1 C11 102.05(15) . . ?
C21 P1 C4 104.23(16) . . ?
C11 P1 C4 103.31(14) . . ?
C21 P1 Mo1 120.49(12) . . ?
C11 P1 Mo1 112.39(11) . . ?
C4 P1 Mo1 112.52(11) . . ?
C41 P2 C31 102.25(15) . . ?
C41 P2 C4 104.07(14) . . ?
C31 P2 C4 104.29(15) . . ?
C41 P2 Mo1 114.14(11) . 2_666 ?
C31 P2 Mo1 121.33(11) . 2_666 ?
C4 P2 Mo1 109.07(11) . 2_666 ?
N1 C1 Mo1 176.7(3) . . ?
N2 C2 Mo1 175.0(3) . . ?
N3 C3 Mo1 165.7(3) . . ?
N3 C3 Mo1 82.2(2) . 2_666 ?
Mo1 C3 Mo1 84.25(12) . 2_666 ?
P1 C4 P2 112.03(16) . . ?
C16 C11 C12 117.9(3) . . ?
C16 C11 P1 123.0(3) . . ?
C12 C11 P1 118.9(3) . . ?
C11 C12 C13 120.5(4) . . ?
C14 C13 C12 120.7(4) . . ?
C15 C14 C13 119.4(4) . . ?
C14 C15 C16 120.1(4) . . ?
C11 C16 C15 121.4(4) . . ?
C26 C21 C22 119.2(3) . . ?
C26 C21 P1 121.0(3) . . ?
C22 C21 P1 119.8(3) . . ?
C23 C22 C21 119.6(4) . . ?
C24 C23 C22 120.1(4) . . ?
C25 C24 C23 121.3(4) . . ?
C24 C25 C26 119.3(4) . . ?
C21 C26 C25 120.4(4) . . ?
C36 C31 C32 119.6(3) . . ?
C36 C31 P2 120.0(3) . . ?
C32 C31 P2 120.4(3) . . ?
C31 C32 C33 119.4(4) . . ?
C34 C33 C32 120.9(4) . . ?
C35 C34 C33 119.5(4) . . ?
C34 C35 C36 120.6(4) . . ?
C31 C36 C35 120.0(4) . . ?
C42 C41 C46 118.7(3) . . ?
C42 C41 P2 124.7(3) . . ?
C46 C41 P2 116.5(3) . . ?
C41 C42 C43 120.5(3) . . ?
C44 C43 C42 120.2(4) . . ?
C45 C44 C43 119.9(4) . . ?
C44 C45 C46 120.5(4) . . ?
C45 C46 C41 120.3(4) . . ?
C3 N3 Mo1 70.4(2) . 2_666 ?
O1 N50 O2 127.5(11) . . ?
O1 N50 C50 125.5(10) . . ?
O2 N50 C50 107.1(9) . . ?
O3 C51 O4 128.2(7) . . ?
O3 C51 N51 116.6(8) . 2_556 ?
O4 C51 N51 113.9(8) . 2_556 ?
O3 C51 C51 116.6(8) . 2_556 ?
O4 C51 C51 113.9(8) . 2_556 ?
N51 C51 C51 0.0(8) 2_556 2_556 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C3 2.087(4) . ?
Mo1 C1 2.176(4) . ?
Mo1 C2 2.251(3) . ?
Mo1 C3 2.284(3) 2_666 ?
Mo1 N3 2.404(3) 2_666 ?
Mo1 P1 2.5474(13) . ?
Mo1 P2 2.5569(14) 2_666 ?
Mo1 Mo1 2.9357(9) 2_666 ?
P1 C21 1.836(3) . ?
P1 C11 1.838(3) . ?
P1 C4 1.851(3) . ?
P2 C41 1.834(3) . ?
P2 C31 1.843(3) . ?
P2 C4 1.856(3) . ?
P2 Mo1 2.5569(14) 2_666 ?
C1 N1 1.127(4) . ?
C2 N2 1.086(4) . ?
C3 N3 1.121(4) . ?
C3 Mo1 2.284(3) 2_666 ?
C11 C16 1.374(5) . ?
C11 C12 1.378(5) . ?
C12 C13 1.393(6) . ?
C13 C14 1.368(7) . ?
C14 C15 1.357(6) . ?
C15 C16 1.393(5) . ?
C21 C26 1.392(5) . ?
C21 C22 1.405(5) . ?
C22 C23 1.389(6) . ?
C23 C24 1.375(7) . ?
C24 C25 1.370(7) . ?
C25 C26 1.397(5) . ?
C31 C36 1.394(5) . ?
C31 C32 1.399(5) . ?
C32 C33 1.401(6) . ?
C33 C34 1.386(7) . ?
C34 C35 1.378(6) . ?
C35 C36 1.399(5) . ?
C41 C42 1.378(5) . ?
C41 C46 1.398(5) . ?
C42 C43 1.407(5) . ?
C43 C44 1.373(6) . ?
C44 C45 1.372(5) . ?
C45 C46 1.394(5) . ?
N3 Mo1 2.402(3) 2_666 ?
C50 N50 1.439(12) . ?
N50 O1 1.118(8) . ?
N50 O2 1.175(12) . ?
C51 O3 1.171(8) . ?
C51 O4 1.351(9) . ?
C51 N51 1.442(11) 2_556 ?
C51 C51 1.442(11) 2_556 ?
