Steric Switching From Photochemical to Thermal Reaction Pathways for Enhanced Efficiency in Metal-Mediated Nitrogen Fixation.
Duman, Leila M.; Farrell, Wesley S.; Zavalij, Peter Y.; Sita, Lawrence R.; Journal of the American Chemical Society  (2016) –; doi:10.1021/jacs.6b09789

data_4125307
_publ_section_title
;
 Steric Switching From Photochemical to Thermal Reaction Pathways for
 Enhanced Efficiency in Metal-Mediated Nitrogen Fixation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.6b09789
_journal_year                    2016
_chemical_formula_moiety         'C21 H30 Cl Mo N3'
_chemical_formula_sum            'C21 H30 Cl Mo N3'
_chemical_formula_weight         455.87
_chemical_name_systematic        Mo-complex
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 96.6010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8041(7)
_cell_length_b                   8.5331(5)
_cell_length_c                   19.6219(11)
_cell_measurement_reflns_used    12251
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      2.5
_cell_volume                     2129.7(2)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0008228
_diffrn_orient_matrix_UB_12      0.0808100
_diffrn_orient_matrix_UB_13      0.0368289
_diffrn_orient_matrix_UB_21      0.0781167
_diffrn_orient_matrix_UB_22      -0.0086290
_diffrn_orient_matrix_UB_23      0.0101805
_diffrn_orient_matrix_UB_31      0.0088012
_diffrn_orient_matrix_UB_32      0.0844213
_diffrn_orient_matrix_UB_33      -0.0342301
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34617
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.090
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_id                LD-2-98
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.481
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         6189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0100P)^2^+2.9560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5288
_reflns_number_total             6189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09789_si_002.cif
_cod_data_source_block           cmpd_7
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4125307
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              60602
_shelx_hkl_checksum              94318