Synthesis and Characterization of Pincer-Molybdenum Precatalysts for CO2Hydrogenation
Zhang, Yuanyuan; Williard, Paul G.; Bernskoetter, Wesley H.; Organometallics 35 (2016) 860–; doi:10.1021/acs.organomet.5b00955

data_4086393
_publ_section_title
;
 Synthesis and Characterization of Pincer-Molybdenum Precatalysts for
 CO2Hydrogenation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              860
_journal_paper_doi               10.1021/acs.organomet.5b00955
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C33 H39 Mo N P2'
_chemical_formula_weight         607.53
_chemical_name_common            wb27may2
_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   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3171(7)
_cell_length_b                   15.3059(11)
_cell_length_c                   18.2283(13)
_cell_measurement_reflns_used    5776
_cell_measurement_temperature    183.(2)
_cell_measurement_theta_max      17.4370
_cell_measurement_theta_min      2.2684
_cell_volume                     2878.5(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      183.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11497
_diffrn_reflns_theta_full        17.44
_diffrn_reflns_theta_max         17.44
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light gold-yellow'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.154
_refine_ls_abs_structure_details
;
Flack x determined using 690 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         1811
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0353P)^2^+1.1041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                1708
_reflns_number_total             1811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00955_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4086393--4086394.cif.'
_cod_database_code               4086393
_shelx_res_checksum              36337
_shelx_hkl_checksum              97797