Mechanistic studies on C–C reductive coupling of five-coordinate Rh(iii) complexes
Chen, Shanshan; Su, Yan; Han, Keli; Li, Xingwei; Organic Chemistry Frontiers 2 (2015) 783–; doi:10.1039/C5QO00049A

data_1553111
_publ_section_title
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 Mechanistic studies on C--C reductive coupling of five-coordinate Rh(iii)
 complexes
;
_journal_issue                   7
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              783
_journal_paper_doi               10.1039/C5QO00049A
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C61 H49 N Rh, 2(C2 H6 O2), F6 P'
_chemical_formula_sum            'C65 H61 F6 N O2 P3 Rh'
_chemical_formula_weight         1197.97
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-06-15 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                75.156(2)
_cell_angle_beta                 79.856(2)
_cell_angle_gamma                69.201(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8319(4)
_cell_length_b                   13.2288(4)
_cell_length_c                   22.0889(8)
_cell_measurement_reflns_used    8456
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2847.44(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66048
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.8770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.233
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         10559
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+10.3968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                8986
_reflns_number_total             10559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qo00049a2.cif
_cod_data_source_block           lxw43
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2847.44(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1553111