Selective C-H Activation at a Molecular Rhodium Sigma-Alkane Complex by Solid/Gas Single-Crystal to Single-Crystal H/D Exchange.
Chadwick, F. Mark; Krämer, Tobias; Gutmann, Torsten; Rees, Nicholas H.; Thompson, Amber L.; Edwards, Alison J.; Buntkowsky, Gerd; Macgregor, Stuart A.; Weller, Andrew S.; Journal of the American Chemical Society 138 (2016) 13369–13378; doi:10.1021/jacs.6b07968

data_4130936
_publ_section_title
;
 Selective C-H Activation at a Molecular Rhodium Sigma-Alkane Complex by
 Solid/Gas Single-Crystal to Single-Crystal H/D Exchange.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13369
_journal_page_last               13378
_journal_paper_doi               10.1021/jacs.6b07968
_journal_volume                  138
_journal_year                    2016
_chemical_compound_source        SYN
_chemical_formula_moiety         'C65 H70 B1 F24 P2 Rh1'
_chemical_formula_sum            'C65 H70 B F24 P2 Rh'
_chemical_formula_weight         1482.89
_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_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-12
_audit_creation_method           CRYSTALS_ver_14.61_build_5555
_cell_angle_alpha                93.895(3)
_cell_angle_beta                 91.116(3)
_cell_angle_gamma                94.190(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8281(7)
_cell_length_b                   13.1804(7)
_cell_length_c                   19.8019(6)
_cell_measurement_reflns_used    8007
_cell_measurement_temperature    150
_cell_measurement_theta_max      74
_cell_measurement_theta_min      3
_cell_volume                     3330.4(3)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24745
_diffrn_reflns_theta_full        68.411
_diffrn_reflns_theta_max         74.360
_diffrn_reflns_theta_min         3.370
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.480
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            clear_pale_orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512.000
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.95
_refine_diff_density_min         -1.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1220
_refine_ls_number_reflns         13096
_refine_ls_number_restraints     2535
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.1059
_refine_ls_shift/su_max          0.0055261
_refine_ls_shift/su_mean         0.0002029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.12P)^2^ +23.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2826
_refine_ls_wR_factor_gt          0.2648
_refine_ls_wR_factor_ref         0.2826
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10275
_reflns_number_total             13152
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.14
_oxford_diffrn_Wilson_scale      0.17
_oxford_refine_ls_r_factor_ref   0.1228
_oxford_refine_ls_scale          3.07(6)
_oxford_reflns_number_all        13096
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 203fmc14
_cod_data_source_file            ja6b07968_si_003.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C65 H70 B1 F24 P2 Rh1'
_cod_database_code               4130936