Solid-State Synthesis and Characterization of σ-Alkane Complexes, [Rh(L2)(η(2),η(2)-C7H12)][BAr(F)4] (L2 = Bidentate Chelating Phosphine).
Pike, Sebastian D.; Chadwick, F. Mark; Rees, Nicholas H.; Scott, Mark P.; Weller, Andrew S.; Krämer, Tobias; Macgregor, Stuart A.; Journal of the American Chemical Society 137 (2015) 820–833; doi:10.1021/ja510437p

data_4123241
_publ_section_title
;
 Solid-State Synthesis and Characterization of \s-Alkane Complexes,
 [Rh(L2)(\h(2),\h(2)-C7H12)][BAr(F)4] (L2 = Bidentate Chelating
 Phosphine).
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              820
_journal_page_last               833
_journal_paper_doi               10.1021/ja510437p
_journal_volume                  137
_journal_year                    2015
_chemical_compound_source        'S10 Lab'
_chemical_formula_moiety         'C32 H12 B F24, C21 H40 P2 Rh'
_chemical_formula_sum            'C53 H52 B F24 P2 Rh'
_chemical_formula_weight         1320.61
_chemical_melting_point          ?
_chemical_name_systematic        '[Rh(dippe)NBD][BArF4]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-05-28
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 100.0884(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.6257(4)
_cell_length_b                   12.85990(10)
_cell_length_c                   24.1810(3)
_cell_measurement_reflns_used    12832
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     11213.2(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22737
_diffrn_reflns_theta_full        25.526
_diffrn_reflns_theta_max         27.448
_diffrn_reflns_theta_min         5.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.09
_refine_diff_density_min         -0.98
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9358
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         12695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0019147
_refine_ls_shift/su_mean         0.0000567
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +35.94P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1099
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1099
_reflns_limit_h_max              46
_reflns_limit_h_min              -47
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                9412
_reflns_number_total             12695
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.54
_oxford_diffrn_Wilson_scale      238.46
_oxford_refine_ls_r_factor_ref   0.0717
_oxford_refine_ls_scale          0.067008(9)
_oxford_reflns_number_all        12695
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 004SDP12
_cod_data_source_file            ja510437p_si_001.cif
_cod_data_source_block           '[3-NBD][BArF4]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4123238--4123246.cif.
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C53 H52 B1 F24 P2 Rh1'
_cod_database_code               4123241
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
VIBR 0, 0.01 = F(471) TO F(480) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;