Diamagnetic molybdenum nitride complexes supported by diligating tripodal triamido-phosphine ligands as precursors to paramagnetic phosphine donors.
Hatnean, Jillian A.; Johnson, Samuel A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14925–14936; doi:10.1039/c5dt01415h

data_7035997
_publ_section_title
;
 Diamagnetic molybdenum nitride complexes supported by diligating tripodal
 triamido-phosphine ligands as precursors to paramagnetic phosphine
 donors.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14925
_journal_page_last               14936
_journal_paper_doi               10.1039/c5dt01415h
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C216  H272  Mo4 N16 Ni1  P4  V4'
_chemical_formula_sum            'C216 H272 Mo4 N16 Ni P4 V4'
_chemical_formula_weight         3862.77
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      82
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'direct - structure invariant direct methods'
_atom_sites_solution_secondary   'direct - structure invariant direct methods'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-04-09T16:41:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-07-20 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.779(6)
_cell_length_b                   26.779(6)
_cell_length_c                   21.946(5)
_cell_measurement_reflns_used    8952
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.58
_cell_measurement_theta_min      2.17
_cell_measurement_wavelength     0.71073
_cell_volume                     15738(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.755
_diffrn_measured_fraction_theta_max 0.755
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.1878
_diffrn_reflns_Laue_measured_fraction_full 0.755
_diffrn_reflns_Laue_measured_fraction_max 0.755
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18286
_diffrn_reflns_point_group_measured_fraction_full 0.648
_diffrn_reflns_point_group_measured_fraction_max 0.648
_diffrn_reflns_theta_full        24.986
_diffrn_reflns_theta_max         24.986
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2014'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    0.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.391
_refine_diff_density_min         -2.325
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details
;
 Flack x determined using 1368 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     455
_refine_ls_number_reflns         8946
_refine_ls_number_restraints     885
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.2776
_refine_ls_R_factor_gt           0.185
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1393P)^2^+961.0591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4578
_refine_ls_wR_factor_ref         0.5056
_reflns_Friedel_coverage         0.667
_reflns_Friedel_fraction_full    0.535
_reflns_Friedel_fraction_max     0.534
_reflns_number_gt                5068
_reflns_number_total             8946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01415h1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7035997--7036004.cif.'
_cod_original_cell_volume        15737(8)
_cod_original_formula_sum        'C216 H272 Mo4 N16 Ni1 P4 V4'
_cod_database_code               7035997
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.942