Conversion of Carbon Dioxide to Methanol Using a C-H Activated Bis(imino)pyridine Molybdenum Hydroboration Catalyst.
Pal, Raja; Groy, Thomas L.; Trovitch, Ryan J.; Inorganic chemistry 54 (2015) 7506–7515; doi:10.1021/acs.inorgchem.5b01102

data_4344019
_publ_section_title
;
 Conversion of Carbon Dioxide to Methanol Using a C-H Activated
 Bis(imino)pyridine Molybdenum Hydroboration Catalyst.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7506
_journal_page_last               7515
_journal_paper_doi               10.1021/acs.inorgchem.5b01102
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '2(C39 H41 Mo N3 P2), C7 H7'
_chemical_formula_sum            'C85 H89 Mo2 N6 P4'
_chemical_formula_weight         1510.38
_chemical_name_common            K6Ph2PPrPDIMoH
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.129(4)
_cell_angle_beta                 82.476(3)
_cell_angle_gamma                76.341(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3197(12)
_cell_length_b                   13.0922(15)
_cell_length_c                   14.2479(17)
_cell_measurement_reflns_used    3985
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      23.5586
_cell_measurement_theta_min      2.3061
_cell_volume                     1839.2(4)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19605
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Bruker Kappa APEX II Duo'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             785
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.628
_refine_diff_density_min         -1.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      11.227
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0164P)^2^+20.1603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                4261
_reflns_number_total             6213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01102_si_002.cif
_cod_data_source_block           K6Ph2PPrPDIMoH
_cod_depositor_comments
'Adding full bibliography for 4344018--4344019.cif.'
_cod_database_code               4344019
_shelx_res_checksum              21561
_shelx_hkl_checksum              99832