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_4125303
_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         'C42 H60 Mo2 N6, C5 H12'
_chemical_formula_sum            'C47 H72 Mo2 N6'
_chemical_formula_weight         912.98
_chemical_name_systematic        Mo-complex
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                61.9968(12)
_cell_angle_beta                 86.9618(13)
_cell_angle_gamma                82.3284(12)
_cell_formula_units_Z            1
_cell_length_a                   9.0973(6)
_cell_length_b                   12.1312(8)
_cell_length_c                   12.6499(8)
_cell_measurement_reflns_used    10739
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      30.9
_cell_measurement_theta_min      2.8
_cell_volume                     1221.50(14)
_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      240(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      0.0297691
_diffrn_orient_matrix_UB_12      -0.0674418
_diffrn_orient_matrix_UB_13      0.0824492
_diffrn_orient_matrix_UB_21      0.0097001
_diffrn_orient_matrix_UB_22      -0.0643613
_diffrn_orient_matrix_UB_23      -0.0290476
_diffrn_orient_matrix_UB_31      0.1064113
_diffrn_orient_matrix_UB_32      0.0126539
_diffrn_orient_matrix_UB_33      -0.0193856
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19881
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             480
_exptl_crystal_id                LD-2-68
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.050
_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     233
_refine_ls_number_reflns         5607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_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^+1.2070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4917
_reflns_number_total             5607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09789_si_002.cif
_cod_data_source_block           cmpd_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4125303
_shelx_estimated_absorpt_t_min   0.763
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              83336
_shelx_hkl_checksum              47273
_shelx_fab_checksum              53848