Hydrodebromination of allylic and benzylic bromides with water catalyzed by a rhodium porphyrin complex.
Yang, Wu; Chen, Chen; Chan, Kin Shing; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12879–12883; doi:10.1039/c8dt02168f

data_7047279
_publ_section_title
;
 Hydrodebromination of allylic and benzylic bromides with water catalyzed
 by a rhodium porphyrin complex.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12879
_journal_page_last               12883
_journal_paper_doi               10.1039/c8dt02168f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'2(C48.72 H38.16 Br N4 O0.72 Rh), C49 H39 Br N4 O Rh'
_chemical_formula_sum            'C146.44 H115.31 Br3 N12 O2.44 Rh3'
_chemical_formula_weight         2630.59
_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   geom
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-16 deposited with the CCDC.
2018-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                97.727(2)
_cell_angle_beta                 102.976(2)
_cell_angle_gamma                97.590(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4853(8)
_cell_length_b                   12.4928(9)
_cell_length_c                   23.5322(17)
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      27.521
_cell_measurement_theta_min      2.379
_cell_volume                     3214.0(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      301.91
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            117626
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         2.657
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0933 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.7837.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1337
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.522
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         11583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0252P)^2^+11.1970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10354
_reflns_number_total             11583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02168f2.cif
_cod_data_source_block           p_sq
_cod_depositor_comments
'Adding full bibliography for 7047279--7047280.cif.'
_cod_database_code               7047279
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.547
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Br1')=FVAR(1)
 Fixed Sof: Br2(0.5) C88(0.5) H88A(0.5) H88B(0.5) H88C(0.5) O1(0.5)
 C0AA(0.71901) H0AA(0.71901) H0AB(0.71901) H0AC(0.71901) O2(0.71901)
3.a Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C), C57(H57A,H57B,
 H57C), C77(H77A,H77B,H77C), C87(H87A,H87B,H87C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C35(H35), C36(H36),
  C42(H42), C43(H43), C45(H45), C46(H46), C52(H52), C53(H53), C55(H55),
 C56(H56), C62(H62), C63(H63), C67(H67), C68(H68), C72(H72), C73(H73), C75(H75),
  C76(H76), C82(H82), C83(H83), C85(H85), C86(H86)
3.c Idealised Me refined as rotating group:
 C88(H88A,H88B,H88C), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              61615
_shelx_fab_checksum              9925
_olex2_submission_special_instructions 'No special instructions were received'