Molybdenum(0) Dinitrogen Complexes Supported by Pentadentate Tetrapodal Phosphine Ligands: Structure, Synthesis, and Reactivity toward Acids.
Hinrichsen, Svea; Kindjajev, Andrei; Adomeit, Sven; Krahmer, Jan; Näther, Christian; Tuczek, Felix; Inorganic chemistry 55 (2016) 8712–8722; doi:10.1021/acs.inorgchem.6b01255

data_4348503
_publ_section_title
;
 Molybdenum(0) Dinitrogen Complexes Supported by Pentadentate Tetrapodal
 Phosphine Ligands: Structure, Synthesis, and Reactivity toward Acids.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8712
_journal_page_last               8722
_journal_paper_doi               10.1021/acs.inorgchem.6b01255
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C39 H53 Mo N2 P5'
_chemical_formula_weight         800.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 107.059(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1665(14)
_cell_length_b                   9.4485(5)
_cell_length_c                   21.9647(14)
_cell_measurement_reflns_used    32837
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.003
_cell_measurement_theta_min      1.242
_cell_volume                     3802.7(4)
_computing_cell_refinement       'X-Area (STOE, 2010)'
_computing_data_collection       'X-Area (STOE, 2010)'
_computing_data_reduction        'X-Area (STOE, 2010)'
_computing_molecular_graphics    'XP and Diamond'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32837
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_min         1.242
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.8529
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape(STOE, 2008)'
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0543
_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/[\s^2^(Fo^2^)+(0.0491P)^2^+0.7082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4910
_reflns_number_total             6707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01255_si_002.cif
_cod_data_source_block           felix136a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4348503
_shelxl_version_number           2014-3
_shelx_res_checksum              16053
_shelx_hkl_checksum              49277