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_7021816
_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, Universtity of Oxford'
_chemical_formula_moiety         'C84 H104 B2 Cl16 P4 Rh2, 3.10(C H2 Cl2)'
_chemical_formula_sum            'C87.1 H110.2 B2 Cl22.2 P4 Rh2'
_chemical_formula_weight         2295.84
_chemical_melting_point          ?
_chemical_name_systematic        '[Rh(dibpe)Cl{C6ClH3(B(ArCl)3)}]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             13-03-18
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                78.048(2)
_cell_angle_beta                 88.4952(19)
_cell_angle_gamma                77.569(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2301(3)
_cell_length_b                   17.4742(5)
_cell_length_c                   23.2939(5)
_cell_measurement_reflns_used    27687
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     5144.0(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_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  0.028
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            54944
_diffrn_reflns_theta_full        74.368
_diffrn_reflns_theta_max         76.668
_diffrn_reflns_theta_min         3.421
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.813
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2340.614
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.035
_platon_squeeze_details
; 
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         3.17
_refine_diff_density_min         -1.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1110
_refine_ls_number_reflns         21268
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.0163011
_refine_ls_shift/su_mean         0.0001459
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +16.61P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1381
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1381
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                18963
_reflns_number_total             21352
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      0.33
_oxford_refine_ls_r_factor_ref   0.0585
_oxford_refine_ls_scale          1.707(6)
_oxford_reflns_number_all        21268
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 051SDP12
_cod_data_source_file            c3dt51617b.txt
_cod_data_source_block           Compound3
_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7021816
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(-2001,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) H   (  13,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,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) H   (  53,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,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) H   ( 113,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   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,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   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,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) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,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) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,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   (  48,X'S) H   ( 481,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   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   ( 201,X'S) H   (2011,X'S) H   (2012,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) H   (2042,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) H   (2072,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) H   (2102,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) H   (2132,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME  C(201)  CL(202)  CL(203)  AND 
CONT  C(201)  CL(203)  CL(202)  AND 
CONT  C(204)  CL(205)  CL(206)  AND 
CONT  C(204)  CL(206)  CL(205)  AND 
CONT  C(207)  CL(208)  CL(209)  AND 
CONT  C(207)  CL(209)  CL(208)  AND 
CONT  C(210)  CL(211)  CL(212)  AND 
CONT  C(210)  CL(212)  CL(211)  AND 
CONT  C(213)  CL(214)  CL(215)  AND 
CONT  C(213)  CL(215)  CL(214) 
SIMU 0.01  C(201)  CL(202)  CL(203)  AND 
CONT  C(201)  CL(203)  CL(202)  AND 
CONT  C(204)  CL(205)  CL(206)  AND 
CONT  C(204)  CL(206)  CL(205)  AND 
CONT  C(207)  CL(208)  CL(209)  AND 
CONT  C(207)  CL(209)  CL(208)  AND 
CONT  C(210)  CL(211)  CL(212)  AND 
CONT  C(210)  CL(212)  CL(211)  AND 
CONT  C(213)  CL(214)  CL(215)  AND 
CONT  C(213)  CL(215)  CL(214) 
DELU 0.01  C(201)  CL(202)  CL(203)  AND 
CONT  C(201)  CL(203)  CL(202)  AND 
CONT  C(204)  CL(205)  CL(206)  AND 
CONT  C(204)  CL(206)  CL(205)  AND 
CONT  C(207)  CL(208)  CL(209)  AND 
CONT  C(207)  CL(209)  CL(208)  AND 
CONT  C(210)  CL(211)  CL(212)  AND 
CONT  C(210)  CL(212)  CL(211)  AND 
CONT  C(213)  CL(214)  CL(215)  AND 
CONT  C(213)  CL(215)  CL(214) 
END                                                                             
;