Base-Promoted, Aerobic, and Regioselective Carbon‒Hydrogen Bond Activation of Thiophene with Group 9 Metalloporphyrins
Yang, Wu; Zhang, Haojie; Li, Liuxiao; Tam, Chun Meng; Feng, Shiyu; Wong, Ka Lai; Lai, Wai Yan; Ng, Sheung Hei; Chen, Chen; Chan, Kin Shing; Organometallics 35 (2016) 3295–; doi:10.1021/acs.organomet.6b00490

data_4088851
_publ_section_title
;
 Base-Promoted, Aerobic, and Regioselective Carbon--Hydrogen Bond
 Activation of Thiophene with Group 9 Metalloporphyrins
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3295
_journal_paper_doi               10.1021/acs.organomet.6b00490
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C53 H41 Cl2 N4 Rh S'
_chemical_formula_weight         939.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                66.9469(17)
_cell_angle_beta                 88.931(2)
_cell_angle_gamma                82.2159(19)
_cell_formula_units_Z            2
_cell_length_a                   9.4863(4)
_cell_length_b                   14.4891(5)
_cell_length_c                   16.7008(6)
_cell_measurement_reflns_used    156
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     2091.23(14)
_computing_cell_refinement       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_collection       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_reduction        'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25258
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.168
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+3.1246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6364
_reflns_number_total             7458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00490_si_002.cif
_cod_data_source_block           WYL3
_cod_database_code               4088851
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.884
_shelxl_version_number           2014/6
_shelx_res_checksum              64858
_shelx_hkl_checksum              69650