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_4344018
_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_sum            'C39 H41 I2 Mo N3 P2'
_chemical_formula_weight         963.43
_chemical_name_common            Ph2PPrPDIMoI2
_chemical_name_systematic        Ph2PPrPDIMoI2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.270(5)
_cell_length_b                   18.930(10)
_cell_length_c                   19.310(10)
_cell_measurement_reflns_used    5245
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      23.8834
_cell_measurement_theta_min      2.2461
_cell_volume                     3754(3)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2013.6-2 (Bruker-AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29746
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    2.111
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear dark red-orange'
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.748
_refine_diff_density_min         -0.608
_refine_ls_abs_structure_details
;
Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                5607
_reflns_number_total             6929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01102_si_002.cif
_cod_data_source_block           Ph2PPrPDIMoI2
_cod_depositor_comments
'Adding full bibliography for 4344018--4344019.cif.'
_cod_original_cell_volume        3754.(3)
_cod_database_code               4344018
_shelx_res_checksum              56716
_shelx_hkl_checksum              54527