C-Cl activation of the weakly coordinating anion [B(3,5-Cl2C6H3)4](-) at a Rh(i) centre in solution and the solid-state.
Pike, Sebastian D.; Weller, Andrew S.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12832–12835; doi:10.1039/c3dt51617b

data_7021813
_publ_section_title
;
 C-Cl activation of the weakly coordinating anion [B(3,5-Cl2C6H3)4](-) at
 a Rh(i) centre in solution and the solid-state.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12832
_journal_page_last               12835
_journal_paper_doi               10.1039/c3dt51617b
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'Lab S10'
_chemical_formula_moiety         'C57.13 H59.27 B1 Br1 Cl2.27 F24 P2 Rh1'
_chemical_formula_sum            'C57.13 H59.27 B Br Cl2.27 F24 P2 Rh'
_chemical_formula_weight         1537.98
_chemical_melting_point          ?
_chemical_name_systematic        '[Rh(dibpe)Br(C6H5)]2[BArF4]2'
_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     other
_audit_creation_date             13-07-08
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                73.8487(16)
_cell_angle_beta                 88.5368(15)
_cell_angle_gamma                87.5505(11)
_cell_formula_units_Z            2
_cell_length_a                   13.4344(4)
_cell_length_b                   16.2486(5)
_cell_length_c                   16.3500(5)
_cell_measurement_reflns_used    14578
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3424.70(18)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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  0.066
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27223
_diffrn_reflns_theta_full        25.856
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         5.120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1543.335
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.91
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9485
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         10296
_refine_ls_number_restraints     569
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.0347177
_refine_ls_shift/su_mean         0.0004073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +16.36P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1498
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1498
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              -19
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7971
_reflns_number_total             15564
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      100.63
_oxford_refine_ls_r_factor_ref   0.0826
_oxford_refine_ls_scale          0.15277(8)
_oxford_reflns_number_all        10296
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 053SDP12
_cod_data_source_file            c3dt51617b.txt
_cod_data_source_block           compound6
_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.

'_atom_sites_solution_primary'
value 'Other' changed to 'other' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C57.13 H59.27 B1 Br1 Cl2.27 F24 P2 Rh1'
_cod_database_code               7021813
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C(100,U'S) C(150,U'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   (  72,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   (  92,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 113,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 151,X'S) H   ( 153,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   ( 172,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 202,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 233,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) H   (1002,X'S) 
RIDE C   ( 150,X'S) H   (1502,X'S) H   (1501,X'S) 
RIDE C   ( 200,X'S) H   (2001,X'S) H   (2002,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(53) C(56) F(220) F(230) F(241) AND 
CONT C(53) C(56) F(230) F(241) F(220) AND 
CONT C(53) C(56) F(241) F(220) F(230) AND 
CONT C(53) C(56) F(221) F(231) F(240) AND 
CONT C(53) C(56) F(231) F(240) F(221) AND 
CONT C(53) C(56) F(240) F(221) F(231) 
DELU 0.015 C(53) C(56) F(220) F(230) F(241) AND 
CONT C(53) C(56) F(230) F(241) F(220) AND 
CONT C(53) C(56) F(241) F(220) F(230) AND 
CONT C(53) C(56) F(221) F(231) F(240) AND 
CONT C(53) C(56) F(231) F(240) F(221) AND 
CONT C(53) C(56) F(240) F(221) F(231) 
SIMU 0.015 C(53) C(56) F(220) F(230) F(241) AND 
CONT C(53) C(56) F(230) F(241) F(220) AND 
CONT C(53) C(56) F(241) F(220) F(230) AND 
CONT C(53) C(56) F(221) F(231) F(240) AND 
CONT C(53) C(56) F(231) F(240) F(221) AND 
CONT C(53) C(56) F(240) F(221) F(231) 
SAME C(43) C(47) F(71) F(81) F(90) AND 
CONT C(43) C(47) F(81) F(90) F(71) AND 
CONT C(43) C(47) F(90) F(71) F(81) AND 
CONT C(43) C(47) F(70) F(80) F(91) AND 
CONT C(43) C(47) F(80) F(91) F(70) AND 
CONT C(43) C(47) F(91) F(70) F(80) 
DELU 0.015 C(43) C(47) F(71) F(81) F(90) AND 
CONT C(43) C(47) F(81) F(90) F(71) AND 
CONT C(43) C(47) F(90) F(71) F(81) AND 
CONT C(43) C(47) F(70) F(80) F(91) AND 
CONT C(43) C(47) F(80) F(91) F(70) AND 
CONT C(43) C(47) F(91) F(70) F(80) 
SIMU 0.015 C(43) C(47) F(71) F(81) F(90) AND 
CONT C(43) C(47) F(81) F(90) F(71) AND 
CONT C(43) C(47) F(90) F(71) F(81) AND 
CONT C(43) C(47) F(70) F(80) F(91) AND 
CONT C(43) C(47) F(80) F(91) F(70) AND 
CONT C(43) C(47) F(91) F(70) F(80) 
SAME CL(100) C(100) CL(101) AND 
CONT CL(100) C(150) CL(150) 
SAME CL(200) C(200) CL(201) AND 
CONT CL(201) C(200) CL(200) 
DELU 0.015 CL(100) C(100) CL(101) AND 
CONT CL(100) C(150) CL(150) 
DELU 0.015 CL(200) C(200) CL(201) AND 
CONT CL(201) C(200) CL(200) 
SIMU 0.01 CL(100) C(100) CL(101) AND 
CONT CL(100) C(150) CL(150) 
SIMU 0.005 CL(200) C(200) CL(201) AND 
CONT CL(201) C(200) CL(200) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = CL(100) TO C(150) 
VIBR .0, 0.00200 = CL(100) TO C(100) 
VIBR .0, 0.00200 = C(100) TO CL(101) 
VIBR .0, 0.00500 = CL(101) TO CL(100) 
VIBR .0, 0.00200 = C(150) TO CL(150) 
VIBR .0, 0.00500 = CL(150) TO CL(100) 
VIBR .0, 0.00200 = C(200) TO CL(200) 
VIBR .0, 0.00200 = C(200) TO CL(201) 
VIBR .0, 0.00500 = CL(201) TO CL(200) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = CL(100) TO C(150) 
U(IJ) .0, 0.04000 = CL(100) TO C(100) 
U(IJ) .0, 0.08000 = C(100) TO CL(101) 
U(IJ) .0, 0.08000 = C(150) TO CL(150) 
U(IJ) .0, 0.08000 = C(200) TO CL(200) 
U(IJ) .0, 0.08000 = C(200) TO CL(201) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;