Terpyridine Molybdenum Dinitrogen Chemistry: Synthesis of Dinitrogen Complexes That Vary by Five Oxidation States.
Bezdek, Máté J; Guo, Sheng; Chirik, Paul J.; Inorganic chemistry 55 (2016) 3117–3127; doi:10.1021/acs.inorgchem.6b00053

data_4347352
_publ_section_title
;
 Terpyridine Molybdenum Dinitrogen Chemistry: Synthesis of Dinitrogen
 Complexes That Vary by Five Oxidation States.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3117
_journal_page_last               3127
_journal_paper_doi               10.1021/acs.inorgchem.6b00053
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C47 H41 Cl Mo N3 P2'
_chemical_formula_weight         841.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-26 # Formatted by publCIF
;
_cell_angle_alpha                74.947(5)
_cell_angle_beta                 75.928(5)
_cell_angle_gamma                79.839(5)
_cell_formula_units_Z            2
_cell_length_a                   12.5590(10)
_cell_length_b                   12.7306(10)
_cell_length_c                   13.1308(11)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.82
_cell_measurement_theta_min      3.56
_cell_volume                     1952.1(3)
_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 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49914
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.213
_diffrn_reflns_theta_min         3.563
_exptl_absorpt_coefficient_mu    4.444
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.1228
_exptl_crystal_size_mid          0.0867
_exptl_crystal_size_min          0.0645
_refine_diff_density_max         2.530
_refine_diff_density_min         -2.048
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+29.3052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5311
_reflns_number_total             6885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00053_si_002.cif
_cod_data_source_block           mb14
_cod_database_code               4347352
_shelxl_version_number           2014-3
_shelx_res_checksum              61375
_shelx_hkl_checksum              20037