Formation of Alkanes by Aerobic Carbon‒Carbon Bond Coupling Reactions Catalyzed by a Phosphovanadomolybdic Acid
Somekh, Miriam; Cohen, Hagai; Diskin-Posner, Yael; Shimon, Linda J. W.; Carmieli, Raanan; Rosenberg, Jeffrey N.; Neumann, Ronny; ACS Catalysis  (2017) 2725–; doi:10.1021/acscatal.7b00461

data_4514170
_publ_section_title
;
 Formation of Alkanes by Aerobic Carbon--Carbon Bond Coupling Reactions
 Catalyzed by a Phosphovanadomolybdic Acid
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2725
_journal_paper_doi               10.1021/acscatal.7b00461
_journal_year                    2017
_chemical_formula_moiety         'C34 H30 Co N4, Cl O4'
_chemical_formula_sum            'C34 H30 Cl Co N4 O4'
_chemical_formula_weight         653.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0978(5)
_cell_length_b                   15.1411(5)
_cell_length_c                   22.9374(7)
_cell_measurement_reflns_used    74464
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.78
_cell_volume                     5938.0(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'Collect package APEX2'
_computing_data_reduction        APEX2
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II KappaCCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.690
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.7162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+4.1383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6245
_reflns_number_total             7389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b00461_si_003.cif
_cod_data_source_block           n544
_cod_database_code               4514170
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.716
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              13546
_shelx_hkl_checksum              6197