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_4123245
_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_absolute_configuration unk
_chemical_compound_source        'S10, CRL, Uni Oxford'
_chemical_formula_moiety         'C49 H50 B1 Cl2 F24.00 P2 Rh1'
_chemical_formula_sum            'C49 H50 B Cl2 F24 P2 Rh'
_chemical_formula_weight         1341.46
_chemical_melting_point          ?
_chemical_name_systematic        '[Rh(dippp)DCE][BArF4]'
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-24
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.90210(10)
_cell_length_b                   12.90210(10)
_cell_length_c                   67.9669(10)
_cell_measurement_reflns_used    9631
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     11314.1(2)
_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_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.971
_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  0.105
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            65822
_diffrn_reflns_theta_full        68.571
_diffrn_reflns_theta_max         77.046
_diffrn_reflns_theta_min         3.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.877
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5392.001
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.24
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1427
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         8542
_refine_ls_number_restraints     2050
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.1153
_refine_ls_shift/su_max          0.0100963
_refine_ls_shift/su_mean         0.0001683
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2697
_refine_ls_wR_factor_gt          0.2600
_refine_ls_wR_factor_ref         0.2697
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              81
_reflns_limit_l_min              0
_reflns_number_gt                6941
_reflns_number_total             11533
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.82
_oxford_diffrn_Wilson_scale      1.08
_oxford_refine_ls_r_factor_ref   0.1317
_oxford_refine_ls_scale          1.034(6)
_oxford_reflns_number_all        8542
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 080SDP13
_cod_data_source_file            ja510437p_si_001.cif
_cod_data_source_block           '[4-DCE][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 41 21 2 '
_cod_original_formula_sum        'C49 H50 B1 Cl2 F24.00 P2 Rh1'
_cod_database_code               4123245
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  73,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  83,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 133,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 143,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 173,X'S) H   ( 172,X'S) H   ( 171,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) H   (1012,X'S) 
RIDE C   ( 2,X'S) H   (1022,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1032,X'S) H   (1031,X'S) 
RIDE C   ( 1,X'S) H   (1001,X'S) H   (1002,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(24) C(27) F(101) F(111) F(120) AND 
CONT C(24) C(27) F(111) F(120) F(101) AND 
CONT C(24) C(27) F(120) F(101) F(111) AND 
CONT C(24) C(27) F(100) F(110) F(121) AND 
CONT C(24) C(27) F(110) F(121) F(100) AND 
CONT C(24) C(27) F(121) F(100) F(110) 
DELU 0.015 C(24) C(27) F(101) F(111) F(120) AND 
CONT C(24) C(27) F(111) F(120) F(101) AND 
CONT C(24) C(27) F(120) F(101) F(111) AND 
CONT C(24) C(27) F(100) F(110) F(121) AND 
CONT C(24) C(27) F(110) F(121) F(100) AND 
CONT C(24) C(27) F(121) F(100) F(110) 
SIMU 0.015 C(24) C(27) F(101) F(111) F(120) AND 
CONT C(24) C(27) F(111) F(120) F(101) AND 
CONT C(24) C(27) F(120) F(101) F(111) AND 
CONT C(24) C(27) F(100) F(110) F(121) AND 
CONT C(24) C(27) F(110) F(121) F(100) AND 
CONT C(24) C(27) F(121) F(100) F(110) 
SAME C(41) C(43) F(220) F(230) F(241) AND 
CONT C(41) C(43) F(230) F(241) F(220) AND 
CONT C(41) C(43) F(241) F(220) F(230) AND 
CONT C(41) C(43) F(221) F(231) F(240) AND 
CONT C(41) C(43) F(231) F(240) F(221) AND 
CONT C(41) C(43) F(240) F(221) F(231) 
DELU 0.015 C(41) C(43) F(220) F(230) F(241) AND 
CONT C(41) C(43) F(230) F(241) F(220) AND 
CONT C(41) C(43) F(241) F(220) F(230) AND 
CONT C(41) C(43) F(221) F(231) F(240) AND 
CONT C(41) C(43) F(231) F(240) F(221) AND 
CONT C(41) C(43) F(240) F(221) F(231) 
SIMU 0.015 C(41) C(43) F(220) F(230) F(241) AND 
CONT C(41) C(43) F(230) F(241) F(220) AND 
CONT C(41) C(43) F(241) F(220) F(230) AND 
CONT C(41) C(43) F(221) F(231) F(240) AND 
CONT C(41) C(43) F(231) F(240) F(221) AND 
CONT C(41) C(43) F(240) F(221) F(231) 
SAME C(32) C(35) F(160) F(170) F(181) AND 
CONT C(32) C(35) F(170) F(181) F(160) AND 
CONT C(32) C(35) F(181) F(160) F(170) AND 
CONT C(32) C(35) F(161) F(171) F(180) AND 
CONT C(32) C(35) F(171) F(180) F(161) AND 
CONT C(32) C(35) F(180) F(161) F(171) 
DELU 0.015 C(32) C(35) F(160) F(170) F(181) AND 
CONT C(32) C(35) F(170) F(181) F(160) AND 
CONT C(32) C(35) F(181) F(160) F(170) AND 
CONT C(32) C(35) F(161) F(171) F(180) AND 
CONT C(32) C(35) F(171) F(180) F(161) AND 
CONT C(32) C(35) F(180) F(161) F(171) 
SIMU 0.015 C(32) C(35) F(160) F(170) F(181) AND 
CONT C(32) C(35) F(170) F(181) F(160) AND 
CONT C(32) C(35) F(181) F(160) F(170) AND 
CONT C(32) C(35) F(161) F(171) F(180) AND 
CONT C(32) C(35) F(171) F(180) F(161) AND 
CONT C(32) C(35) F(180) F(161) F(171) 
SAME C(48) C(51) F(310) F(321) F(331) AND 
CONT C(48) C(51) F(321) F(331) F(310) AND 
CONT C(48) C(51) F(331) F(310) F(321) AND 
CONT C(48) C(51) F(311) F(320) F(330) AND 
CONT C(48) C(51) F(320) F(330) F(311) AND 
CONT C(48) C(51) F(330) F(311) F(320) 
DELU 0.015 C(48) C(51) F(310) F(321) F(331) AND 
CONT C(48) C(51) F(321) F(331) F(310) AND 
CONT C(48) C(51) F(331) F(310) F(321) AND 
CONT C(48) C(51) F(311) F(320) F(330) AND 
CONT C(48) C(51) F(320) F(330) F(311) AND 
CONT C(48) C(51) F(330) F(311) F(320) 
SIMU 0.015 C(48) C(51) F(310) F(321) F(331) AND 
CONT C(48) C(51) F(321) F(331) F(310) AND 
CONT C(48) C(51) F(331) F(310) F(321) AND 
CONT C(48) C(51) F(311) F(320) F(330) AND 
CONT C(48) C(51) F(320) F(330) F(311) AND 
CONT C(48) C(51) F(330) F(311) F(320) 
SAME C(46) C(50) F(280) F(290) F(300) AND 
CONT C(46) C(50) F(290) F(300) F(280) AND 
CONT C(46) C(50) F(300) F(280) F(290) AND 
CONT C(46) C(50) F(281) F(291) F(301) AND 
CONT C(46) C(50) F(291) F(301) F(281) AND 
CONT C(46) C(50) F(301) F(281) F(291) 
DELU 0.015 C(46) C(50) F(280) F(290) F(300) AND 
CONT C(46) C(50) F(290) F(300) F(280) AND 
CONT C(46) C(50) F(300) F(280) F(290) AND 
CONT C(46) C(50) F(281) F(291) F(301) AND 
CONT C(46) C(50) F(291) F(301) F(281) AND 
CONT C(46) C(50) F(301) F(281) F(291) 
SIMU 0.015 C(46) C(50) F(280) F(290) F(300) AND 
CONT C(46) C(50) F(290) F(300) F(280) AND 
CONT C(46) C(50) F(300) F(280) F(290) AND 
CONT C(46) C(50) F(281) F(291) F(301) AND 
CONT C(46) C(50) F(291) F(301) F(281) AND 
CONT C(46) C(50) F(301) F(281) F(291) 
SAME C(30) C(34) F(191) F(201) F(210) AND 
CONT C(30) C(34) F(201) F(210) F(191) AND 
CONT C(30) C(34) F(210) F(191) F(201) AND 
CONT C(30) C(34) F(190) F(200) F(211) AND 
CONT C(30) C(34) F(200) F(211) F(190) AND 
CONT C(30) C(34) F(211) F(190) F(200) 
DELU 0.015 C(30) C(34) F(191) F(201) F(210) AND 
CONT C(30) C(34) F(201) F(210) F(191) AND 
CONT C(30) C(34) F(210) F(191) F(201) AND 
CONT C(30) C(34) F(190) F(200) F(211) AND 
CONT C(30) C(34) F(200) F(211) F(190) AND 
CONT C(30) C(34) F(211) F(190) F(200) 
SIMU 0.015 C(30) C(34) F(191) F(201) F(210) AND 
CONT C(30) C(34) F(201) F(210) F(191) AND 
CONT C(30) C(34) F(210) F(191) F(201) AND 
CONT C(30) C(34) F(190) F(200) F(211) AND 
CONT C(30) C(34) F(200) F(211) F(190) AND 
CONT C(30) C(34) F(211) F(190) F(200) 
SAME C(38) C(42) F(250) F(261) F(270) AND 
CONT C(38) C(42) F(261) F(270) F(250) AND 
CONT C(38) C(42) F(270) F(250) F(261) AND 
CONT C(38) C(42) F(251) F(260) F(271) AND 
CONT C(38) C(42) F(260) F(271) F(251) AND 
CONT C(38) C(42) F(271) F(251) F(260) 
DELU 0.015 C(38) C(42) F(250) F(261) F(270) AND 
CONT C(38) C(42) F(261) F(270) F(250) AND 
CONT C(38) C(42) F(270) F(250) F(261) AND 
CONT C(38) C(42) F(251) F(260) F(271) AND 
CONT C(38) C(42) F(260) F(271) F(251) AND 
CONT C(38) C(42) F(271) F(251) F(260) 
SIMU 0.015 C(38) C(42) F(250) F(261) F(270) AND 
CONT C(38) C(42) F(261) F(270) F(250) AND 
CONT C(38) C(42) F(270) F(250) F(261) AND 
CONT C(38) C(42) F(251) F(260) F(271) AND 
CONT C(38) C(42) F(260) F(271) F(251) AND 
CONT C(38) C(42) F(271) F(251) F(260) 
SAME C(44) C(45) C(46) C(47) C(48) C(49) AND 
CONT C(45) C(46) C(47) C(48) C(49) C(44) AND 
CONT C(46) C(47) C(48) C(49) C(44) C(45) AND 
CONT C(47) C(48) C(49) C(44) C(45) C(46) AND 
CONT C(48) C(49) C(44) C(45) C(46) C(47) AND 
CONT C(49) C(44) C(45) C(46) C(47) C(48) 
DELU 0.015 C(44) C(45) C(46) C(47) C(48) C(49) AND 
CONT C(45) C(46) C(47) C(48) C(49) C(44) AND 
CONT C(46) C(47) C(48) C(49) C(44) C(45) AND 
CONT C(47) C(48) C(49) C(44) C(45) C(46) AND 
CONT C(48) C(49) C(44) C(45) C(46) C(47) AND 
CONT C(49) C(44) C(45) C(46) C(47) C(48) 
SIMU 0.015 C(44) C(45) C(46) C(47) C(48) C(49) AND 
CONT C(45) C(46) C(47) C(48) C(49) C(44) AND 
CONT C(46) C(47) C(48) C(49) C(44) C(45) AND 
CONT C(47) C(48) C(49) C(44) C(45) C(46) AND 
CONT C(48) C(49) C(44) C(45) C(46) C(47) AND 
CONT C(49) C(44) C(45) C(46) C(47) C(48) 
PLANAR 0.010000 C(44) C(45) C(46) C(47) C(48) C(49) 
SAME RH(1) CL(1) C(1) C(2) CL(2) AND 
CONT RH(1) CL(2) C(2) C(1) CL(1) AND 
CONT RH(1) CL(10) C(101) C(103) CL(20) AND 
CONT RH(1) CL(20) C(103) C(101) CL(10) 
SIMU 0.01 CL(1) C(1) C(2) CL(2) AND 
CONT CL(2) C(2) C(1) CL(1) AND 
CONT CL(10) C(101) C(103) CL(20) AND 
CONT CL(20) C(103) C(101) CL(10) 
DELU 0.01 CL(1) C(1) C(2) CL(2) AND 
CONT CL(2) C(2) C(1) CL(1) AND 
CONT CL(10) C(101) C(103) CL(20) AND 
CONT CL(20) C(103) C(101) CL(10) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;