#------------------------------------------------------------------------------
#$Date: 2023-07-05 11:45:30 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/92/1569254.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_1569254
loop_
_publ_author_name
'Jin, Li'
'Zhang, Guoqiang'
'Yang, Xiaoqin'
'Song, Jinyi'
'Wang, Jin'
'Liao, Qian'
_publ_section_title
;
 A synthetic cycle for iminophosphorane synthesis involving direct
 intermolecular NP bond formation on N₂-derived
 molybdenum nitride.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7955
_journal_page_last               7958
_journal_paper_doi               10.1039/d3cc01925j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         C18H33I3MoN2P2,NaC14H28O6,C4H8O
_chemical_formula_sum            'C36 H69 I3 Mo N2 Na O7 P2'
_chemical_formula_weight         1203.50
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1871(3)
_cell_length_b                   18.9167(5)
_cell_length_c                   22.6936(6)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.58
_cell_measurement_theta_min      3.04
_cell_volume                     4802.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0319
_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       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73210
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.041
_exptl_absorpt_coefficient_mu    18.437
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             2388
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, diethylether'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.026(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0220
_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)+(0.0305P)²+1.6459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8206
_reflns_number_total             8405
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc01925j2.cif
_cod_data_source_block           MoI3Na
_cod_depositor_comments
'Adding full bibliography for 1569251--1569256.cif.'
_cod_database_code               1569254
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.216
_shelx_estimated_absorpt_t_max   0.320
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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_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
I1 I 0.53802(3) 0.77268(2) 0.37414(2) 0.02900(8) Uani 1 1 d . . . . .
I2 I 0.49786(3) 0.90610(2) 0.23975(2) 0.03198(8) Uani 1 1 d . . . . .
I3 I 0.73547(3) 0.78569(2) 0.14889(2) 0.03085(8) Uani 1 1 d . . . . .
Mo1 Mo 0.63564(3) 0.78012(2) 0.26150(2) 0.01915(8) Uani 1 1 d . . . . .
P1 P 0.82926(11) 0.82962(6) 0.30260(5) 0.0236(2) Uani 1 1 d . . . . .
P2 P 0.49413(11) 0.68208(6) 0.23029(5) 0.0238(2) Uani 1 1 d . . . . .
N2 N 0.5701(4) 0.6105(2) 0.25399(18) 0.0252(9) Uani 1 1 d . . . . .
H2A H 0.5363 0.5686 0.2526 0.030 Uiso 1 1 calc R U . . .
C1 C 0.7355(4) 0.6857(2) 0.28226(19) 0.0204(9) Uani 1 1 d . . . . .
C6 C 0.6874(4) 0.6175(2) 0.2760(2) 0.0208(9) Uani 1 1 d . . . . .
N1 N 0.9069(4) 0.7546(2) 0.31464(19) 0.0273(9) Uani 1 1 d . . . . .
H1A H 0.9812 0.7568 0.3273 0.033 Uiso 1 1 calc R U . . .
C5 C 0.7499(4) 0.5563(2) 0.2914(2) 0.0236(9) Uani 1 1 d . . . . .
H5A H 0.7129 0.5113 0.2882 0.028 Uiso 1 1 calc R U . . .
C13 C 0.3490(5) 0.6733(3) 0.2680(3) 0.0393(13) Uani 1 1 d . . . . .
H13A H 0.3699 0.6765 0.3108 0.047 Uiso 1 1 calc R U . . .
C4 C 0.8661(5) 0.5621(3) 0.3112(2) 0.0288(11) Uani 1 1 d . . . . .
H4A H 0.9099 0.5205 0.3205 0.035 Uiso 1 1 calc R U . . .
C3 C 0.9197(4) 0.6279(3) 0.3177(2) 0.0262(10) Uani 1 1 d . . . . .
H3A H 1.0002 0.6316 0.3308 0.031 Uiso 1 1 calc R U . . .
C16 C 0.4744(5) 0.6674(3) 0.1499(3) 0.0354(12) Uani 1 1 d . . . . .
H16A H 0.5571 0.6684 0.1331 0.042 Uiso 1 1 calc R U . . .
C2 C 0.8534(4) 0.6886(2) 0.3046(2) 0.0215(9) Uani 1 1 d . . . . .
C7 C 0.8200(5) 0.8737(3) 0.3754(3) 0.0340(12) Uani 1 1 d . . . . .
H7A H 0.7753 0.8400 0.4012 0.041 Uiso 1 1 calc R U . . .
C9 C 0.7434(6) 0.9400(3) 0.3730(3) 0.0461(15) Uani 1 1 d . . . . .
H9A H 0.6684 0.9295 0.3525 0.069 Uiso 1 1 calc R U . . .
H9B H 0.7258 0.9559 0.4132 0.069 Uiso 1 1 calc R U . . .
H9C H 0.7865 0.9772 0.3519 0.069 Uiso 1 1 calc R U . . .
C11 C 1.0559(5) 0.8904(3) 0.2711(3) 0.0417(14) Uani 1 1 d . . . . .
H11A H 1.0896 0.8450 0.2836 0.063 Uiso 1 1 calc R U . . .
H11B H 1.1030 0.9094 0.2383 0.063 Uiso 1 1 calc R U . . .
H11C H 1.0579 0.9237 0.3042 0.063 Uiso 1 1 calc R U . . .
C17 C 0.4092(7) 0.7285(4) 0.1203(3) 0.0566(18) Uani 1 1 d . . . . .
H17A H 0.4445 0.7733 0.1330 0.085 Uiso 1 1 calc R U . . .
H17B H 0.4166 0.7241 0.0774 0.085 Uiso 1 1 calc R U . . .
H17C H 0.3245 0.7273 0.1313 0.085 Uiso 1 1 calc R U . . .
O7 O 0.7615(7) 0.3863(3) 0.4701(3) 0.087(2) Uani 1 1 d . U . . .
C33 C 0.806(5) 0.331(4) 0.493(4) 0.086(4) Uani 0.272(13) 1 d D U P A 1
H33A H 0.7580 0.2894 0.4824 0.103 Uiso 0.272(13) 1 calc R U P A 1
H33B H 0.8047 0.3358 0.5369 0.103 Uiso 0.272(13) 1 calc R U P A 1
C34 C 0.931(4) 0.321(2) 0.473(2) 0.090(4) Uani 0.272(13) 1 d D U P A 1
H34A H 0.9837 0.3133 0.5078 0.108 Uiso 0.272(13) 1 calc R U P A 1
H34B H 0.9359 0.2792 0.4474 0.108 Uiso 0.272(13) 1 calc R U P A 1
C35 C 0.969(3) 0.3821(19) 0.4422(17) 0.091(4) Uani 0.272(13) 1 d D U P A 1
H35A H 0.9861 0.3702 0.4006 0.109 Uiso 0.272(13) 1 calc R U P A 1
H35B H 1.0416 0.4022 0.4603 0.109 Uiso 0.272(13) 1 calc R U P A 1
C36 C 0.872(4) 0.4317(19) 0.4456(18) 0.089(4) Uani 0.272(13) 1 d D U P A 1
H36A H 0.8537 0.4516 0.4062 0.107 Uiso 0.272(13) 1 calc R U P A 1
H36B H 0.8917 0.4709 0.4728 0.107 Uiso 0.272(13) 1 calc R U P A 1
C33' C 0.8325(19) 0.3284(14) 0.4924(13) 0.084(3) Uani 0.728(13) 1 d D U P A 2
H33C H 0.7874 0.2835 0.4897 0.101 Uiso 0.728(13) 1 calc R U P A 2
H33D H 0.8541 0.3367 0.5341 0.101 Uiso 0.728(13) 1 calc R U P A 2
C34' C 0.9419(18) 0.3251(10) 0.4552(7) 0.091(3) Uani 0.728(13) 1 d D U P A 2
H34C H 1.0070 0.3535 0.4728 0.109 Uiso 0.728(13) 1 calc R U P A 2
H34D H 0.9696 0.2756 0.4508 0.109 Uiso 0.728(13) 1 calc R U P A 2
C35' C 0.9071(15) 0.3532(9) 0.4003(6) 0.091(3) Uani 0.728(13) 1 d D U P A 2
H35C H 0.8885 0.3146 0.3724 0.109 Uiso 0.728(13) 1 calc R U P A 2
H35D H 0.9725 0.3822 0.3835 0.109 Uiso 0.728(13) 1 calc R U P A 2
C36' C 0.8017(14) 0.3967(7) 0.4101(5) 0.077(3) Uani 0.728(13) 1 d D U P A 2
H36C H 0.8213 0.4472 0.4035 0.092 Uiso 0.728(13) 1 calc R U P A 2
H36D H 0.7376 0.3831 0.3822 0.092 Uiso 0.728(13) 1 calc R U P A 2
C10 C 0.9281(5) 0.8798(3) 0.2514(3) 0.0347(12) Uani 1 1 d . . . . .
H10A H 0.9337 0.8497 0.2153 0.042 Uiso 1 1 calc R U . . .
C12 C 0.8676(5) 0.9478(3) 0.2311(3) 0.0431(15) Uani 1 1 d . . . . .
H12A H 0.7853 0.9375 0.2189 0.065 Uiso 1 1 calc R U . . .
H12B H 0.8667 0.9820 0.2635 0.065 Uiso 1 1 calc R U . . .
H12C H 0.9118 0.9677 0.1977 0.065 Uiso 1 1 calc R U . . .
C15 C 0.2860(6) 0.6035(4) 0.2628(4) 0.0534(17) Uani 1 1 d . . . . .
H15A H 0.3431 0.5651 0.2695 0.080 Uiso 1 1 calc R U . . .
H15B H 0.2220 0.6009 0.2922 0.080 Uiso 1 1 calc R U . . .
H15C H 0.2517 0.5990 0.2232 0.080 Uiso 1 1 calc R U . . .
C18 C 0.4229(6) 0.5961(4) 0.1314(3) 0.0478(15) Uani 1 1 d . . . . .
H18A H 0.4668 0.5581 0.1513 0.072 Uiso 1 1 calc R U . . .
H18B H 0.3383 0.5938 0.1426 0.072 Uiso 1 1 calc R U . . .
H18C H 0.4304 0.5906 0.0887 0.072 Uiso 1 1 calc R U . . .
C14 C 0.2662(6) 0.7352(4) 0.2581(4) 0.060(2) Uani 1 1 d . . . . .
H14A H 0.3112 0.7794 0.2619 0.090 Uiso 1 1 calc R U . . .
H14B H 0.2317 0.7322 0.2185 0.090 Uiso 1 1 calc R U . . .
H14C H 0.2020 0.7342 0.2874 0.090 Uiso 1 1 calc R U . . .
C8 C 0.9374(6) 0.8874(4) 0.4069(3) 0.0494(16) Uani 1 1 d . . . . .
H8A H 0.9848 0.8438 0.4078 0.074 Uiso 1 1 calc R U . . .
H8B H 0.9820 0.9243 0.3860 0.074 Uiso 1 1 calc R U . . .
H8C H 0.9213 0.9029 0.4474 0.074 Uiso 1 1 calc R U . . .
Na1 Na 0.6305(2) 0.46228(13) 0.51609(9) 0.0406(5) Uani 1 1 d D . . . .
O2 O 0.4347(5) 0.4704(3) 0.4748(2) 0.0652(15) Uani 1 1 d . . . . .
O3 O 0.5007(6) 0.3824(3) 0.5653(2) 0.0610(13) Uani 1 1 d . . . . .
O4 O 0.6529(5) 0.4738(3) 0.6202(2) 0.0529(11) Uani 1 1 d . . . . .
O5 O 0.7618(5) 0.5591(3) 0.5389(2) 0.0636(14) Uani 1 1 d . . . . .
O6 O 0.6302(6) 0.5425(4) 0.4385(3) 0.0775(18) Uani 1 1 d . . . . .
C23 C 0.3747(6) 0.4049(5) 0.4817(4) 0.075(3) Uani 1 1 d D . . . .
H23A H 0.4123 0.3684 0.4565 0.089 Uiso 1 1 calc R U . . .
H23B H 0.2899 0.4097 0.4700 0.089 Uiso 1 1 calc R U . . .
C24 C 0.3835(8) 0.3837(5) 0.5462(5) 0.072(3) Uani 1 1 d . . . . .
H24A H 0.3375 0.4176 0.5705 0.086 Uiso 1 1 calc R U . . .
H24B H 0.3477 0.3363 0.5516 0.086 Uiso 1 1 calc R U . . .
C25 C 0.5126(9) 0.3800(4) 0.6271(4) 0.065(2) Uani 1 1 d . . . . .
H25A H 0.5011 0.3308 0.6408 0.078 Uiso 1 1 calc R U . . .
H25B H 0.4498 0.4096 0.6454 0.078 Uiso 1 1 calc R U . . .
C26 C 0.6336(8) 0.4059(4) 0.6464(3) 0.0593(19) Uani 1 1 d D . . . .
H26A H 0.6367 0.4097 0.6899 0.071 Uiso 1 1 calc R U . . .
H26B H 0.6964 0.3725 0.6335 0.071 Uiso 1 1 calc R U . . .
C27 C 0.7681(8) 0.5008(5) 0.6329(3) 0.065(2) Uani 1 1 d D . . . .
H27A H 0.8304 0.4668 0.6204 0.077 Uiso 1 1 calc R U . . .
H27B H 0.7768 0.5094 0.6757 0.077 Uiso 1 1 calc R U . . .
C28 C 0.7804(8) 0.5694(5) 0.5992(4) 0.065(2) Uani 1 1 d . . . . .
H28A H 0.7216 0.6040 0.6143 0.078 Uiso 1 1 calc R U . . .
H28B H 0.8614 0.5891 0.6056 0.078 Uiso 1 1 calc R U . . .
C29 C 0.7299(9) 0.6196(5) 0.5064(5) 0.083(3) Uani 1 1 d . . . . .
H29A H 0.7948 0.6551 0.5088 0.099 Uiso 1 1 calc R U . . .
H29B H 0.6565 0.6408 0.5232 0.099 Uiso 1 1 calc R U . . .
C30 C 0.7088(9) 0.5997(5) 0.4433(4) 0.072(2) Uani 1 1 d . . . . .
H30A H 0.6753 0.6407 0.4219 0.087 Uiso 1 1 calc R U . . .
H30B H 0.7860 0.5872 0.4247 0.087 Uiso 1 1 calc R U . . .
C31 C 0.5212(9) 0.5583(5) 0.4139(3) 0.073(3) Uani 1 1 d . . . . .
H31A H 0.5318 0.5732 0.3724 0.088 Uiso 1 1 calc R U . . .
H31B H 0.4829 0.5975 0.4358 0.088 Uiso 1 1 calc R U . . .
C32 C 0.4414(9) 0.4910(6) 0.4169(3) 0.075(3) Uani 1 1 d . . . . .
H32A H 0.3605 0.5015 0.4015 0.090 Uiso 1 1 calc R U . . .
H32B H 0.4767 0.4527 0.3927 0.090 Uiso 1 1 calc R U . . .
O1 O 0.0988(4) 0.7264(3) 0.4114(2) 0.0557(11) Uani 1 1 d . U . . .
C19 C 0.0136(7) 0.6980(4) 0.4518(3) 0.0549(14) Uani 1 1 d . U . . .
H19A H -0.0656 0.6938 0.4327 0.066 Uiso 1 1 calc R U . . .
H19B H 0.0058 0.7293 0.4866 0.066 Uiso 1 1 calc R U . . .
C20 C 0.0582(9) 0.6257(6) 0.4705(4) 0.0753(18) Uani 1 1 d . U . . .
H20A H 0.0433 0.6172 0.5129 0.090 Uiso 1 1 calc R U . . .
H20B H 0.0199 0.5877 0.4472 0.090 Uiso 1 1 calc R U . . .
C21 C 0.1872(10) 0.6304(7) 0.4579(6) 0.099(2) Uani 1 1 d . U . . .
H21A H 0.2331 0.6310 0.4952 0.119 Uiso 1 1 calc R U . . .
H21B H 0.2131 0.5888 0.4346 0.119 Uiso 1 1 calc R U . . .
C22 C 0.2090(8) 0.6936(6) 0.4256(5) 0.085(2) Uani 1 1 d . U . . .
H22A H 0.2585 0.7263 0.4494 0.102 Uiso 1 1 calc R U . . .
H22B H 0.2533 0.6824 0.3890 0.102 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
C1 Mo1 P1 77.47(13) . . ?
C1 Mo1 P2 77.27(13) . . ?
P1 Mo1 P2 154.73(4) . . ?
C1 Mo1 I1 87.76(12) . . ?
P1 Mo1 I1 90.91(3) . . ?
P2 Mo1 I1 88.55(3) . . ?
C1 Mo1 I3 91.37(12) . . ?
P1 Mo1 I3 88.91(3) . . ?
P2 Mo1 I3 91.24(3) . . ?
I1 Mo1 I3 179.129(17) . . ?
C1 Mo1 I2 177.14(12) . . ?
P1 Mo1 I2 102.38(3) . . ?
P2 Mo1 I2 102.88(3) . . ?
I1 Mo1 I2 89.385(13) . . ?
I3 Mo1 I2 91.486(14) . . ?
N1 P1 C7 105.3(2) . . ?
N1 P1 C10 103.0(2) . . ?
C7 P1 C10 111.1(3) . . ?
N1 P1 Mo1 100.85(15) . . ?
C7 P1 Mo1 116.47(19) . . ?
C10 P1 Mo1 117.73(19) . . ?
N2 P2 C13 102.9(2) . . ?
N2 P2 C16 104.7(2) . . ?
C13 P2 C16 109.8(3) . . ?
N2 P2 Mo1 100.55(15) . . ?
C13 P2 Mo1 119.1(2) . . ?
C16 P2 Mo1 117.17(18) . . ?
C6 N2 P2 120.5(3) . . ?
C6 N2 H2A 119.8 . . ?
P2 N2 H2A 119.8 . . ?
C6 C1 C2 115.4(4) . . ?
C6 C1 Mo1 122.6(3) . . ?
C2 C1 Mo1 121.9(3) . . ?
C5 C6 C1 123.0(4) . . ?
C5 C6 N2 118.5(4) . . ?
C1 C6 N2 118.5(4) . . ?
C2 N1 P1 120.2(3) . . ?
C2 N1 H1A 119.9 . . ?
P1 N1 H1A 119.9 . . ?
C4 C5 C6 119.2(4) . . ?
C4 C5 H5A 120.4 . . ?
C6 C5 H5A 120.4 . . ?
C15 C13 C14 112.5(5) . . ?
C15 C13 P2 117.2(4) . . ?
C14 C13 P2 113.7(5) . . ?
C15 C13 H13A 103.9 . . ?
C14 C13 H13A 103.9 . . ?
P2 C13 H13A 103.9 . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C4 C3 C2 118.9(5) . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C17 C16 C18 111.6(5) . . ?
C17 C16 P2 112.1(5) . . ?
C18 C16 P2 116.5(4) . . ?
C17 C16 H16A 105.2 . . ?
C18 C16 H16A 105.2 . . ?
P2 C16 H16A 105.2 . . ?
C3 C2 N1 118.0(4) . . ?
C3 C2 C1 122.6(4) . . ?
N1 C2 C1 119.4(4) . . ?
C8 C7 C9 111.3(5) . . ?
C8 C7 P1 116.6(4) . . ?
C9 C7 P1 111.8(4) . . ?
C8 C7 H7A 105.3 . . ?
C9 C7 H7A 105.3 . . ?
P1 C7 H7A 105.3 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C33' O7 C36' 105.2(11) . . ?
C33 O7 C36 106(3) . . ?
C33 O7 Na1 125(3) . . ?
C33' O7 Na1 131.6(11) . . ?
C36' O7 Na1 122.6(6) . . ?
C36 O7 Na1 108.3(12) . . ?
O7 C33 C34 110(3) . . ?
O7 C33 H33A 109.6 . . ?
C34 C33 H33A 109.6 . . ?
O7 C33 H33B 109.6 . . ?
C34 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C35 C34 C33 109(3) . . ?
C35 C34 H34A 109.8 . . ?
C33 C34 H34A 109.8 . . ?
C35 C34 H34B 109.8 . . ?
C33 C34 H34B 109.8 . . ?
H34A C34 H34B 108.3 . . ?
C34 C35 C36 106(2) . . ?
C34 C35 H35A 110.5 . . ?
C36 C35 H35A 110.5 . . ?
C34 C35 H35B 110.5 . . ?
C36 C35 H35B 110.5 . . ?
H35A C35 H35B 108.6 . . ?
C35 C36 O7 104(2) . . ?
C35 C36 H36A 110.9 . . ?
O7 C36 H36A 110.9 . . ?
C35 C36 H36B 110.9 . . ?
O7 C36 H36B 110.9 . . ?
H36A C36 H36B 108.9 . . ?
O7 C33' C34' 106.6(13) . . ?
O7 C33' H33C 110.4 . . ?
C34' C33' H33C 110.4 . . ?
O7 C33' H33D 110.4 . . ?
C34' C33' H33D 110.4 . . ?
H33C C33' H33D 108.6 . . ?
C35' C34' C33' 105.0(15) . . ?
C35' C34' H34C 110.7 . . ?
C33' C34' H34C 110.7 . . ?
C35' C34' H34D 110.7 . . ?
C33' C34' H34D 110.7 . . ?
H34C C34' H34D 108.8 . . ?
C34' C35' C36' 107.6(11) . . ?
C34' C35' H35C 110.2 . . ?
C36' C35' H35C 110.2 . . ?
C34' C35' H35D 110.2 . . ?
C36' C35' H35D 110.2 . . ?
H35C C35' H35D 108.5 . . ?
O7 C36' C35' 108.5(10) . . ?
O7 C36' H36C 110.0 . . ?
C35' C36' H36C 110.0 . . ?
O7 C36' H36D 110.0 . . ?
C35' C36' H36D 110.0 . . ?
H36C C36' H36D 108.4 . . ?
C11 C10 C12 113.4(5) . . ?
C11 C10 P1 116.4(4) . . ?
C12 C10 P1 110.8(4) . . ?
C11 C10 H10A 105.0 . . ?
C12 C10 H10A 105.0 . . ?
P1 C10 H10A 105.0 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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 . . ?
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 . . ?
O7 Na1 O6 93.7(2) . . ?
O7 Na1 O3 101.9(2) . . ?
O6 Na1 O3 140.4(3) . . ?
O7 Na1 O4 116.0(2) . . ?
O6 Na1 O4 133.7(2) . . ?
O3 Na1 O4 69.93(19) . . ?
O7 Na1 O2 116.5(3) . . ?
O6 Na1 O2 70.1(2) . . ?
O3 Na1 O2 70.4(2) . . ?
O4 Na1 O2 118.7(2) . . ?
O7 Na1 O5 100.6(3) . . ?
O6 Na1 O5 70.5(2) . . ?
O3 Na1 O5 139.2(2) . . ?
O4 Na1 O5 69.68(19) . . ?
O2 Na1 O5 126.6(2) . . ?
C32 O2 C23 112.3(7) . . ?
C32 O2 Na1 110.1(5) . . ?
C23 O2 Na1 109.5(5) . . ?
C24 O3 C25 113.7(7) . . ?
C24 O3 Na1 115.0(5) . . ?
C25 O3 Na1 115.6(5) . . ?
C27 O4 C26 112.2(6) . . ?
C27 O4 Na1 109.3(4) . . ?
C26 O4 Na1 108.2(4) . . ?
C28 O5 C29 115.9(7) . . ?
C28 O5 Na1 114.1(5) . . ?
C29 O5 Na1 110.6(6) . . ?
C31 O6 C30 114.9(7) . . ?
C31 O6 Na1 116.8(5) . . ?
C30 O6 Na1 116.4(5) . . ?
O2 C23 C24 107.9(6) . . ?
O2 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
O2 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
O3 C24 C23 111.6(7) . . ?
O3 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
O3 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
O3 C25 C26 111.3(6) . . ?
O3 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
O3 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
O4 C26 C25 107.9(5) . . ?
O4 C26 H26A 110.1 . . ?
C25 C26 H26A 110.1 . . ?
O4 C26 H26B 110.1 . . ?
C25 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
O4 C27 C28 106.9(6) . . ?
O4 C27 H27A 110.3 . . ?
C28 C27 H27A 110.3 . . ?
O4 C27 H27B 110.3 . . ?
C28 C27 H27B 110.3 . . ?
H27A C27 H27B 108.6 . . ?
O5 C28 C27 111.2(7) . . ?
O5 C28 H28A 109.4 . . ?
C27 C28 H28A 109.4 . . ?
O5 C28 H28B 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
O5 C29 C30 109.6(7) . . ?
O5 C29 H29A 109.8 . . ?
C30 C29 H29A 109.8 . . ?
O5 C29 H29B 109.8 . . ?
C30 C29 H29B 109.8 . . ?
H29A C29 H29B 108.2 . . ?
O6 C30 C29 111.6(7) . . ?
O6 C30 H30A 109.3 . . ?
C29 C30 H30A 109.3 . . ?
O6 C30 H30B 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 108.0 . . ?
O6 C31 C32 108.2(7) . . ?
O6 C31 H31A 110.0 . . ?
C32 C31 H31A 110.0 . . ?
O6 C31 H31B 110.0 . . ?
C32 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
O2 C32 C31 107.7(6) . . ?
O2 C32 H32A 110.2 . . ?
C31 C32 H32A 110.2 . . ?
O2 C32 H32B 110.2 . . ?
C31 C32 H32B 110.2 . . ?
H32A C32 H32B 108.5 . . ?
C22 O1 C19 105.7(6) . . ?
O1 C19 C20 107.4(6) . . ?
O1 C19 H19A 110.2 . . ?
C20 C19 H19A 110.2 . . ?
O1 C19 H19B 110.2 . . ?
C20 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
C21 C20 C19 102.3(9) . . ?
C21 C20 H20A 111.3 . . ?
C19 C20 H20A 111.3 . . ?
C21 C20 H20B 111.3 . . ?
C19 C20 H20B 111.3 . . ?
H20A C20 H20B 109.2 . . ?
C22 C21 C20 108.5(9) . . ?
C22 C21 H21A 110.0 . . ?
C20 C21 H21A 110.0 . . ?
C22 C21 H21B 110.0 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
O1 C22 C21 109.6(8) . . ?
O1 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
O1 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
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
I1 Mo1 2.7834(5) . ?
I2 Mo1 2.8808(5) . ?
I3 Mo1 2.7910(5) . ?
Mo1 C1 2.159(4) . ?
Mo1 P1 2.5375(12) . ?
Mo1 P2 2.5391(12) . ?
P1 N1 1.687(4) . ?
P1 C7 1.853(6) . ?
P1 C10 1.863(6) . ?
P2 N2 1.686(4) . ?
P2 C13 1.842(6) . ?
P2 C16 1.859(6) . ?
N2 C6 1.411(6) . ?
N2 H2A 0.8800 . ?
C1 C6 1.406(7) . ?
C1 C2 1.414(7) . ?
C6 C5 1.396(7) . ?
N1 C2 1.402(6) . ?
N1 H1A 0.8800 . ?
C5 C4 1.380(8) . ?
C5 H5A 0.9500 . ?
C13 C15 1.501(9) . ?
C13 C14 1.510(8) . ?
C13 H13A 1.0000 . ?
C4 C3 1.391(8) . ?
C4 H4A 0.9500 . ?
C3 C2 1.399(7) . ?
C3 H3A 0.9500 . ?
C16 C17 1.523(8) . ?
C16 C18 1.526(8) . ?
C16 H16A 1.0000 . ?
C7 C8 1.519(8) . ?
C7 C9 1.520(8) . ?
C7 H7A 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C10 1.511(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O7 C33 1.27(5) . ?
O7 C33' 1.445(19) . ?
O7 C36' 1.447(11) . ?
O7 C36 1.60(4) . ?
O7 Na1 2.303(7) . ?
C33 C34 1.48(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.42(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.43(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C33' C34' 1.487(17) . ?
C33' H33C 0.9900 . ?
C33' H33D 0.9900 . ?
C34' C35' 1.410(19) . ?
C34' H34C 0.9900 . ?
C34' H34D 0.9900 . ?
C35' C36' 1.455(18) . ?
C35' H35C 0.9900 . ?
C35' H35D 0.9900 . ?
C36' H36C 0.9900 . ?
C36' H36D 0.9900 . ?
C10 C12 1.526(8) . ?
C10 H10A 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Na1 O6 2.323(6) . ?
Na1 O3 2.374(6) . ?
Na1 O4 2.387(5) . ?
Na1 O2 2.387(6) . ?
Na1 O5 2.405(6) . ?
O2 C32 1.373(10) . ?
O2 C23 1.418(10) . ?
O3 C24 1.380(11) . ?
O3 C25 1.410(10) . ?
O4 C27 1.415(9) . ?
O4 C26 1.431(8) . ?
O5 C28 1.397(10) . ?
O5 C29 1.408(12) . ?
O6 C31 1.374(11) . ?
O6 C30 1.398(12) . ?
C23 C24 1.521(14) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.505(13) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.512(13) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.500(15) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.557(15) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O1 C22 1.416(11) . ?
O1 C19 1.428(8) . ?
C19 C20 1.515(12) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.475(14) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.425(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 P2 N2 C6 -130.9(4) . . . . ?
C16 P2 N2 C6 114.4(4) . . . . ?
Mo1 P2 N2 C6 -7.6(4) . . . . ?
C2 C1 C6 C5 0.8(7) . . . . ?
Mo1 C1 C6 C5 -177.6(3) . . . . ?
C2 C1 C6 N2 180.0(4) . . . . ?
Mo1 C1 C6 N2 1.6(6) . . . . ?
P2 N2 C6 C5 -175.6(3) . . . . ?
P2 N2 C6 C1 5.1(6) . . . . ?
C7 P1 N1 C2 117.8(4) . . . . ?
C10 P1 N1 C2 -125.8(4) . . . . ?
Mo1 P1 N1 C2 -3.7(4) . . . . ?
C1 C6 C5 C4 -2.9(7) . . . . ?
N2 C6 C5 C4 177.9(4) . . . . ?
N2 P2 C13 C15 -51.0(6) . . . . ?
C16 P2 C13 C15 60.0(6) . . . . ?
Mo1 P2 C13 C15 -161.0(5) . . . . ?
N2 P2 C13 C14 175.1(5) . . . . ?
C16 P2 C13 C14 -73.9(6) . . . . ?
Mo1 P2 C13 C14 65.1(6) . . . . ?
C6 C5 C4 C3 2.0(8) . . . . ?
C5 C4 C3 C2 0.9(8) . . . . ?
N2 P2 C16 C17 -178.7(4) . . . . ?
C13 P2 C16 C17 71.5(5) . . . . ?
Mo1 P2 C16 C17 -68.3(5) . . . . ?
N2 P2 C16 C18 51.0(5) . . . . ?
C13 P2 C16 C18 -58.8(5) . . . . ?
Mo1 P2 C16 C18 161.3(4) . . . . ?
C4 C3 C2 N1 176.4(5) . . . . ?
C4 C3 C2 C1 -3.1(7) . . . . ?
P1 N1 C2 C3 -177.3(4) . . . . ?
P1 N1 C2 C1 2.3(6) . . . . ?
C6 C1 C2 C3 2.2(7) . . . . ?
Mo1 C1 C2 C3 -179.3(4) . . . . ?
C6 C1 C2 N1 -177.3(4) . . . . ?
Mo1 C1 C2 N1 1.1(6) . . . . ?
N1 P1 C7 C8 54.9(5) . . . . ?
C10 P1 C7 C8 -55.9(6) . . . . ?
Mo1 P1 C7 C8 165.6(4) . . . . ?
N1 P1 C7 C9 -175.4(4) . . . . ?
C10 P1 C7 C9 73.8(5) . . . . ?
Mo1 P1 C7 C9 -64.7(5) . . . . ?
C36 O7 C33 C34 -17(8) . . . . ?
Na1 O7 C33 C34 -144(4) . . . . ?
O7 C33 C34 C35 10(9) . . . . ?
C33 C34 C35 C36 3(7) . . . . ?
C34 C35 C36 O7 -12(5) . . . . ?
C33 O7 C36 C35 19(6) . . . . ?
Na1 O7 C36 C35 155(3) . . . . ?
C36' O7 C33' C34' 22(3) . . . . ?
Na1 O7 C33' C34' -149.6(14) . . . . ?
O7 C33' C34' C35' -27(3) . . . . ?
C33' C34' C35' C36' 22(3) . . . . ?
C33' O7 C36' C35' -9(2) . . . . ?
Na1 O7 C36' C35' 163.7(10) . . . . ?
C34' C35' C36' O7 -9(2) . . . . ?
N1 P1 C10 C11 -53.2(5) . . . . ?
C7 P1 C10 C11 59.0(5) . . . . ?
Mo1 P1 C10 C11 -163.0(4) . . . . ?
N1 P1 C10 C12 175.3(4) . . . . ?
C7 P1 C10 C12 -72.5(5) . . . . ?
Mo1 P1 C10 C12 65.4(5) . . . . ?
C32 O2 C23 C24 174.4(8) . . . . ?
Na1 O2 C23 C24 51.6(8) . . . . ?
C25 O3 C24 C23 165.6(7) . . . . ?
Na1 O3 C24 C23 29.1(8) . . . . ?
O2 C23 C24 O3 -54.6(10) . . . . ?
C24 O3 C25 C26 -158.5(7) . . . . ?
Na1 O3 C25 C26 -22.3(8) . . . . ?
C27 O4 C26 C25 -176.3(6) . . . . ?
Na1 O4 C26 C25 -55.7(6) . . . . ?
O3 C25 C26 O4 52.5(9) . . . . ?
C26 O4 C27 C28 175.8(6) . . . . ?
Na1 O4 C27 C28 55.7(7) . . . . ?
C29 O5 C28 C27 158.7(7) . . . . ?
Na1 O5 C28 C27 28.5(9) . . . . ?
O4 C27 C28 O5 -56.7(9) . . . . ?
C28 O5 C29 C30 -177.9(7) . . . . ?
Na1 O5 C29 C30 -46.1(8) . . . . ?
C31 O6 C30 C29 112.2(9) . . . . ?
Na1 O6 C30 C29 -29.7(10) . . . . ?
O5 C29 C30 O6 50.9(11) . . . . ?
C30 O6 C31 C32 -175.2(7) . . . . ?
Na1 O6 C31 C32 -33.4(9) . . . . ?
C23 O2 C32 C31 -173.5(7) . . . . ?
Na1 O2 C32 C31 -51.1(8) . . . . ?
O6 C31 C32 O2 56.6(9) . . . . ?
C22 O1 C19 C20 -26.1(9) . . . . ?
O1 C19 C20 C21 21.9(10) . . . . ?
C19 C20 C21 C22 -9.6(13) . . . . ?
C19 O1 C22 C21 20.1(12) . . . . ?
C20 C21 C22 O1 -6.0(15) . . . . ?
