Heavy metal boryl chemistry: complexes of cadmium, mercury and lead
Andrey V. Protchenko; Deepak Dange; Andrew D. Schwarz; Christina Y. Tang; Nicholas Phillips; Philip Mountford; Cameron Jones; Simon Aldridge; Chem.Commun. 50 (2014) 3841–; doi:10.1039/C4CC00697F

data_7112170
_publ_section_title
;
 Heavy metal boryl chemistry: complexes of cadmium, mercury and lead
;
_journal_name_full               Chem.Commun.
_journal_page_first              3841
_journal_paper_doi               10.1039/C4CC00697F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C52 H72 B2 Hg N4'
_chemical_formula_sum            'C52 H72 B2 Hg N4'
_chemical_formula_weight         975.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-07-11
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 91.0133(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.92100(10)
_cell_length_b                   26.7541(2)
_cell_length_c                   14.71750(10)
_cell_measurement_reflns_used    12182
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     5086.89(6)
_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 0.991
_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  0.021
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61976
_diffrn_reflns_theta_full        27.303
_diffrn_reflns_theta_max         27.860
_diffrn_reflns_theta_min         5.123
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.062
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.270
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       63.363
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         11990
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.0152630
_refine_ls_shift/su_mean         0.0005320
_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: 
 25.3 38.6 22.7 9.65 2.44 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0647
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0647
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                9912
_reflns_number_total             11991
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.90
_oxford_diffrn_Wilson_scale      21.50
_oxford_refine_ls_r_factor_ref   0.0358
_oxford_refine_ls_scale          0.22586(7)
_oxford_reflns_number_all        11991
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 006apct10
_cod_data_source_file            c4cc00697f2.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7112170
_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) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,OCC) 
EQUIV PART(4001,OCC) PART(4002,OCC) 
WEIGHT -1 PART(4002,OCC) 
RIDE C   ( 600,X'S) H   (6001,X'S) 
RIDE C   ( 601,X'S) H   (6012,X'S) H   (6011,X'S) H   (6013,X'S) 
RIDE C   ( 602,X'S) H   (6022,X'S) H   (6021,X'S) H   (6023,X'S) 
RIDE C   ( 610,X'S) H   (6101,X'S) 
RIDE C   ( 611,X'S) H   (6111,X'S) H   (6112,X'S) H   (6113,X'S) 
RIDE C   ( 612,X'S) H   (6121,X'S) H   (6122,X'S) H   (6123,X'S) 
RIDE C   ( 500,X'S) H   (5001,X'S) 
RIDE C   ( 501,X'S) H   (5011,X'S) H   (5013,X'S) H   (5012,X'S) 
RIDE C   ( 502,X'S) H   (5021,X'S) H   (5023,X'S) H   (5022,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) 
RIDE C   ( 511,X'S) H   (5112,X'S) H   (5111,X'S) H   (5113,X'S) 
RIDE C   ( 512,X'S) H   (5121,X'S) H   (5123,X'S) H   (5122,X'S) 
RIDE C   ( 400,X'S) H   (4001,X'S) 
RIDE C   ( 401,X'S) H   (4012,X'S) H   (4011,X'S) H   (4013,X'S) 
RIDE C   ( 402,X'S) H   (4022,X'S) H   (4021,X'S) H   (4023,X'S) 
RIDE C   ( 410,X'S) H   (4101,X'S) 
RIDE C   ( 411,X'S) H   (4111,X'S) H   (4112,X'S) H   (4113,X'S) 
RIDE C   ( 412,X'S) H   (4121,X'S) H   (4122,X'S) H   (4123,X'S) 
RIDE C   ( 300,X'S) H   (3001,X'S) 
RIDE C   ( 301,X'S) H   (3011,X'S) H   (3013,X'S) H   (3012,X'S) 
RIDE C   ( 302,X'S) H   (3021,X'S) H   (3023,X'S) H   (3022,X'S) 
RIDE C   ( 310,X'S) H   (3101,X'S) 
RIDE C   ( 311,X'S) H   (3111,X'S) H   (3113,X'S) H   (3112,X'S) 
RIDE C   ( 312,X'S) H   (3121,X'S) H   (3123,X'S) H   (3122,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,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   ( 122,X'S) H   ( 121,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) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 261,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,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   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME C(53) C(300) C(301) C(302) AND 
CONT C(53) C(300) C(302) C(301) AND 
CONT C(53) C(310) C(311) C(312) AND 
CONT C(53) C(310) C(312) C(311) 
SIMU 0.01 C(53) C(300) C(301) C(302) AND 
CONT C(53) C(300) C(302) C(301) AND 
CONT C(53) C(310) C(311) C(312) AND 
CONT C(53) C(310) C(312) C(311) 
DELU 0.01 C(53) C(300) C(301) C(302) AND 
CONT C(53) C(300) C(302) C(301) AND 
CONT C(53) C(310) C(311) C(312) AND 
CONT C(53) C(310) C(312) C(311) 
SAME C(41) C(400) C(401) C(402) AND 
CONT C(41) C(400) C(402) C(401) AND 
CONT C(41) C(410) C(411) C(412) AND 
CONT C(41) C(410) C(412) C(411) 
SIMU 0.01 C(41) C(400) C(401) C(402) AND 
CONT C(41) C(400) C(402) C(401) AND 
CONT C(41) C(410) C(411) C(412) AND 
CONT C(41) C(410) C(412) C(411) 
DELU 0.01 C(41) C(400) C(401) C(402) AND 
CONT C(41) C(400) C(402) C(401) AND 
CONT C(41) C(410) C(411) C(412) AND 
CONT C(41) C(410) C(412) C(411) 
SAME C(49) C(500) C(501) C(502) AND 
CONT C(49) C(500) C(502) C(501) AND 
CONT C(49) C(510) C(511) C(512) AND 
CONT C(49) C(510) C(512) C(511) 
SIMU 0.01 C(49) C(500) C(501) C(502) AND 
CONT C(49) C(500) C(502) C(501) AND 
CONT C(49) C(510) C(511) C(512) AND 
CONT C(49) C(510) C(512) C(511) 
DELU 0.01 C(49) C(500) C(501) C(502) AND 
CONT C(49) C(500) C(502) C(501) AND 
CONT C(49) C(510) C(511) C(512) AND 
CONT C(49) C(510) C(512) C(511) 
SAME C(37) C(600) C(601) C(602) AND 
CONT C(37) C(600) C(602) C(601) AND 
CONT C(37) C(610) C(611) C(612) AND 
CONT C(37) C(610) C(612) C(611) 
SIMU 0.01 C(37) C(600) C(601) C(602) AND 
CONT C(37) C(600) C(602) C(601) AND 
CONT C(37) C(610) C(611) C(612) AND 
CONT C(37) C(610) C(612) C(611) 
DELU 0.01 C(37) C(600) C(601) C(602) AND 
CONT C(37) C(600) C(602) C(601) AND 
CONT C(37) C(610) C(611) C(612) AND 
CONT C(37) C(610) C(612) C(611) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;