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_7021814
_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        'CRL, University of Oxford'
_chemical_formula_moiety         'C49 H60.00 B1 Cl8 P2 Rh1'
_chemical_formula_sum            'C49 H60 B Cl8 P2 Rh'
_chemical_formula_weight         1108.30
_chemical_melting_point          ?
_chemical_name_systematic        '[RhdibpeNBD][BArCl4]'
_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             13-07-08
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                88.3937(9)
_cell_angle_beta                 89.8872(9)
_cell_angle_gamma                86.3926(9)
_cell_formula_units_Z            2
_cell_length_a                   12.0494(3)
_cell_length_b                   12.4222(3)
_cell_length_c                   17.4694(4)
_cell_measurement_reflns_used    10712
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2608.61(11)
_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  0.038
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20032
_diffrn_reflns_theta_full        25.824
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1140.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.34
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10747
_refine_ls_number_restraints     1312
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.0333983
_refine_ls_shift/su_mean         0.0007767
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +14.62P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1563
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1563
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                8238
_reflns_number_total             11812
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.00
_oxford_diffrn_Wilson_scale      23.11
_oxford_refine_ls_r_factor_ref   0.0870
_oxford_refine_ls_scale          0.21721(13)
_oxford_reflns_number_all        10747
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 031SDP12
_cod_data_source_file            c3dt51617b.txt
_cod_data_source_block           Compound1
_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 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        'C49 H60.00 B1 Cl8 P2 Rh1'
_cod_database_code               7021814
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
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   (  72,X'S) H   (  71,X'S) 
RIDE C   (   8,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   ( 103,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 113,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,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   ( 152,X'S) H   ( 151,X'S) H   ( 153,X'S) 
RIDE C   (  17,X'S) H   ( 172,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 213,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 243,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 261,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   ( 292,X'S) H   ( 291,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 303,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 333,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 343,X'S) H   ( 341,X'S) H   ( 342,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   (  57,X'S) H   ( 571,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) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   ( 161,X'S) H   (1611,X'S) H   (1612,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.01000000 U[ISO] 
LIMIT      0.01000000 X 
LIMIT      0.01000000 Y 
LIMIT      0.01000000 Z 
LIMIT      0.01000000 U[11] 
LIMIT      0.01000000 U[22] 
LIMIT      0.01000000 U[33] 
LIMIT      0.01000000 U[12] 
LIMIT      0.01000000 U[13] 
LIMIT      0.01000000 U[23] 
LIMIT      0.01000000 OCC 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
SAME C(18) C(19) C(20) C(21)  AND 
CONT C(18) C(19) C(21) C(20)  AND 
CONT C(22) C(23) C(24) C(25)  AND 
CONT C(22) C(23) C(25) C(24)  AND 
CONT C(27) C(28) C(29) C(30)  AND 
CONT C(27) C(28) C(30) C(29)  AND 
CONT C(31) C(32) C(33) C(34)  AND 
CONT C(31) C(32) C(34) C(33) 
DELU 0.015 C(18) C(19) C(20) C(21)  AND 
CONT C(18) C(19) C(21) C(20)  AND 
CONT C(22) C(23) C(24) C(25)  AND 
CONT C(22) C(23) C(25) C(24)  AND 
CONT C(27) C(28) C(29) C(30)  AND 
CONT C(27) C(28) C(30) C(29)  AND 
CONT C(31) C(32) C(33) C(34)  AND 
CONT C(31) C(32) C(34) C(33) 
SIMU 0.015 C(18) C(19) C(20) C(21)  AND 
CONT C(18) C(19) C(21) C(20)  AND 
CONT C(22) C(23) C(24) C(25)  AND 
CONT C(22) C(23) C(25) C(24)  AND 
CONT C(27) C(28) C(29) C(30)  AND 
CONT C(27) C(28) C(30) C(29)  AND 
CONT C(31) C(32) C(33) C(34)  AND 
CONT C(31) C(32) C(34) C(33) 
SAME P(1) C(16) C(26) P(3) AND 
CONT P(1) C(161) C(17) P(2) 
DELU 0.02 P(1) C(16) C(26) P(3) AND 
CONT P(1) C(161) C(17) P(2) 
SIMU 0.02 P(1) C(16) C(26) P(3) AND 
CONT P(1) C(161) C(17) P(2) 
SAME C(18) P(2) C(22) AND 
CONT C(22) P(2) C(18) AND 
CONT C(27) P(3) C(31) AND 
CONT C(31) P(3) C(27) 
END                                                                             
;