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_4123240
_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         'C58 H60 B1 F24 P2 Rh1'
_chemical_formula_sum            'C58 H60 B F24 P2 Rh'
_chemical_formula_weight         1388.73
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-13
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 107.0678(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2898(2)
_cell_length_b                   13.03780(10)
_cell_length_c                   26.3494(2)
_cell_measurement_reflns_used    23850
_cell_measurement_temperature    150
_cell_measurement_theta_max      75
_cell_measurement_theta_min      3
_cell_volume                     6006.52(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.984
_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  0.033
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44991
_diffrn_reflns_theta_full        72.048
_diffrn_reflns_theta_max         75.050
_diffrn_reflns_theta_min         3.674
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.816
_exptl_absorpt_correction_T_max  0.47
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         12128
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.0671810
_refine_ls_shift/su_mean         0.0014323
_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: 
 0.112E+04 0.184E+04 0.110E+04 441. 97.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0790
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0789
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                10821
_reflns_number_total             12178
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.95
_oxford_diffrn_Wilson_scale      0.40
_oxford_refine_ls_r_factor_ref   0.0374
_oxford_refine_ls_scale          1.669(4)
_oxford_reflns_number_all        12129
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '202fmc14.cif_od At 16:57 on 25/ 3'
_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) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,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) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,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   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   ( 240,X'S) H   (2401,X'S) H   (2402,X'S) 
RIDE C   ( 241,X'S) H   (2411,X'S) H   (2412,X'S) 
RIDE C   ( 230,X'S) H   (2301,X'S) H   (2302,X'S) 
RIDE C   ( 231,X'S) H   (2311,X'S) H   (2312,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) 
RIDE C   ( 260,X'S) H   (2601,X'S) H   (2602,X'S) 
RIDE C   ( 261,X'S) H   (2611,X'S) H   (2612,X'S) 
RIDE C   ( 250,X'S) H   (2501,X'S) H   (2502,X'S) 
RIDE C   ( 251,X'S) H   (2511,X'S) H   (2512,X'S) 
RIDE C   ( 220,X'S) H   (2201,X'S) H   (2202,X'S) 
RIDE C   ( 221,X'S) H   (2211,X'S) H   (2212,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
SAME C(210) C(220) C(230) C(241) C(251) C(261) AND 
CONT C(210) C(261) C(251) C(241) C(230) C(220) AND 
CONT C(211) C(221) C(231) C(240) C(250) C(260) AND 
CONT C(211) C(260) C(250) C(240) C(231) C(221) 
DELU 0.015 C(210) C(220) C(230) C(241) C(251) C(261) AND 
CONT C(210) C(261) C(251) C(241) C(230) C(220) AND 
CONT C(211) C(221) C(231) C(240) C(250) C(260) AND 
CONT C(211) C(260) C(250) C(240) C(231) C(221) 
SIMU 0.015 C(210) C(220) C(230) C(241) C(251) C(261) AND 
CONT C(210) C(261) C(251) C(241) C(230) C(220) AND 
CONT C(211) C(221) C(231) C(240) C(250) C(260) AND 
CONT C(211) C(260) C(250) C(240) C(231) C(221) 
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-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 21/c 1 '
_cod_original_formula_sum        'C58 H60 B1 F24 P2 Rh1'
_cod_database_code               4123240