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_4123238
_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        SYN
_chemical_formula_moiety         'Rh1 P2 C33 H56; B1 C32 H12 F24'
_chemical_formula_sum            'C65 H68 B F24 P2 Rh'
_chemical_formula_weight         1480.87
_chemical_melting_point          ?
_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             2014-06-17
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                93.0486(19)
_cell_angle_beta                 90.1923(18)
_cell_angle_gamma                96.187(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8259(3)
_cell_length_b                   13.0175(3)
_cell_length_c                   19.8317(4)
_cell_measurement_reflns_used    20648
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     3287.04(13)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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_pressure         101
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_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  0.031
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35636
_diffrn_reflns_theta_full        74.248
_diffrn_reflns_theta_max         76.545
_diffrn_reflns_theta_min         3.420
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.525
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.90
_refine_diff_density_min         -1.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0761
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         13560
_refine_ls_number_restraints     456
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.0051147
_refine_ls_shift/su_mean         0.0001335
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.549E+04 0.912E+04 0.618E+04 0.286E+04 931. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2403
_refine_ls_wR_factor_gt          0.2399
_refine_ls_wR_factor_ref         0.2403
_reflns_limit_h_max              16
_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                12725
_reflns_number_total             13617
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.86
_oxford_diffrn_Wilson_scale      0.16
_oxford_refine_ls_r_factor_ref   0.0815
_oxford_refine_ls_scale          2.70(3)
_oxford_reflns_number_all        13561
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'C:\Users\ASWGroup\Desktop\Crsyta At 16:25 on'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
SAME C(46) C(49) F(100) F(110) F(120) AND 
CONT C(46) C(49) F(110) F(120) F(100) AND 
CONT C(46) C(49) F(120) F(100) F(110) AND 
CONT C(46) C(49) F(101) F(111) F(121) AND 
CONT C(46) C(49) F(111) F(121) F(101) AND 
CONT C(46) C(49) F(121) F(101) F(111) 
DELU 0.015 C(46) C(49) F(100) F(110) F(120) AND 
CONT C(46) C(49) F(110) F(120) F(100) AND 
CONT C(46) C(49) F(120) F(100) F(110) AND 
CONT C(46) C(49) F(101) F(111) F(121) AND 
CONT C(46) C(49) F(111) F(121) F(101) AND 
CONT C(46) C(49) F(121) F(101) F(111) 
SIMU 0.015 C(46) C(49) F(100) F(110) F(120) AND 
CONT C(46) C(49) F(110) F(120) F(100) AND 
CONT C(46) C(49) F(120) F(100) F(110) AND 
CONT C(46) C(49) F(101) F(111) F(121) AND 
CONT C(46) C(49) F(111) F(121) F(101) AND 
CONT C(46) C(49) F(121) F(101) F(111) 
SAME C(44) C(48) F(70) F(80) F(90) AND 
CONT C(44) C(48) F(80) F(90) F(70) AND 
CONT C(44) C(48) F(90) F(70) F(80) AND 
CONT C(44) C(48) F(71) F(81) F(91) AND 
CONT C(44) C(48) F(81) F(91) F(71) AND 
CONT C(44) C(48) F(91) F(71) F(81) 
DELU 0.015 C(44) C(48) F(70) F(80) F(90) AND 
CONT C(44) C(48) F(80) F(90) F(70) AND 
CONT C(44) C(48) F(90) F(70) F(80) AND 
CONT C(44) C(48) F(71) F(81) F(91) AND 
CONT C(44) C(48) F(81) F(91) F(71) AND 
CONT C(44) C(48) F(91) F(71) F(81) 
SIMU 0.015 C(44) C(48) F(70) F(80) F(90) AND 
CONT C(44) C(48) F(80) F(90) F(70) AND 
CONT C(44) C(48) F(90) F(70) F(80) AND 
CONT C(44) C(48) F(71) F(81) F(91) AND 
CONT C(44) C(48) F(81) F(91) F(71) AND 
CONT C(44) C(48) F(91) F(71) F(81) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_cod_data_source_file            ja510437p_si_001.cif
_cod_data_source_block           '[2-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      'P -1 '
_cod_original_formula_sum        'C65 H68 B1 F24 P2 Rh1'
_cod_database_code               4123238