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_4123242
_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, CRL, Uni Oxford'
_chemical_formula_moiety         'C46 H44 B1 F24 P2 Rh1'
_chemical_formula_sum            'C46 H44 B F24 P2 Rh'
_chemical_formula_weight         1228.47
_chemical_melting_point          ?
_chemical_name_systematic        Rh(dippe)(h6-BArF4)
_space_group_IT_number           2
_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             12-05-30
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                67.8471(8)
_cell_angle_beta                 72.8930(7)
_cell_angle_gamma                68.3387(8)
_cell_formula_units_Z            2
_cell_length_a                   12.6227(2)
_cell_length_b                   14.0591(2)
_cell_length_c                   16.1221(3)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2422.52(7)
_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 0.988
_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_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19043
_diffrn_reflns_theta_full        25.238
_diffrn_reflns_theta_max         27.433
_diffrn_reflns_theta_min         5.091
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.85
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9848
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         10921
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.0258628
_refine_ls_shift/su_mean         0.0009386
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 2.80P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0864
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0864
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8562
_reflns_number_total             10921
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.66
_oxford_diffrn_Wilson_scale      21.94
_oxford_refine_ls_r_factor_ref   0.0609
_oxford_refine_ls_scale          0.22439(9)
_oxford_reflns_number_all        10921
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 011SDP12
_cod_data_source_file            ja510437p_si_001.cif
_cod_data_source_block           '[3-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      'P -1 '
_cod_original_formula_sum        'C46 H44 B1 F24 P2 Rh1'
_cod_database_code               4123242
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(43) C(46) F(22) F(24) F(23) AND 
CONT C(43) C(46) F(24) F(23) F(22) AND 
CONT C(43) C(46) F(23) F(22) F(24) AND 
CONT C(43) C(46) F(122) F(124) F(123) AND 
CONT C(43) C(46) F(124) F(123) F(122) AND 
CONT C(43) C(46) F(123) F(122) F(124) 
DELU 0.015 C(43) C(46) F(22) F(24) F(23) AND 
CONT C(43) C(46) F(24) F(23) F(22) AND 
CONT C(43) C(46) F(23) F(22) F(24) AND 
CONT C(43) C(46) F(122) F(124) F(123) AND 
CONT C(43) C(46) F(124) F(123) F(122) AND 
CONT C(43) C(46) F(123) F(122) F(124) 
SIMU 0.015 C(43) C(46) F(22) F(24) F(23) AND 
CONT C(43) C(46) F(24) F(23) F(22) AND 
CONT C(43) C(46) F(23) F(22) F(24) AND 
CONT C(43) C(46) F(122) F(124) F(123) AND 
CONT C(43) C(46) F(124) F(123) F(122) AND 
CONT C(43) C(46) F(123) F(122) F(124) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;