Steric control of the reactivity of moderately hindered tris(pyrazolyl)borates with copper(II) salts †
Chia, Li Mei Lindy; Radojevic, Sanja; Scowen, Ian J.; McPartlin, Mary; Halcrow, Malcolm A.; Journal of the Chemical Society, Dalton Transactions  (2000) 133–; doi:10.1039/a907258f

data_7008945
_publ_section_title
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 Steric control of the reactivity of moderately hindered
 tris(pyrazolyl)borates with copper(II) salts&#x200A;&#x2020;
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_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              133
_journal_paper_doi               10.1039/a907258f
_journal_year                    2000
_chemical_formula_moiety         '[C45 H68 B Cu N10][B F4][C H Cl3]'
_chemical_formula_sum            'C46 H69 B2 Cl3 Cu F4 N10'
_chemical_formula_weight         1029.62
_chemical_name_systematic
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Bis-[5-cyclohexylpyrazole][hydrido-tris-{3-cyclohexylpyrazol-1-yl}borato] 
copper(II) tetrafluoroborate chloroform solvate
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_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.666(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.514(2)
_cell_length_b                   18.291(3)
_cell_length_c                   12.439(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      10.94
_cell_measurement_theta_min      2.72
_cell_volume                     2614.3(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'theta/2 theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3749
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.95510
_exptl_absorpt_correction_T_min  0.21284
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         2582
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.109
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_obs          0.0721
_refine_ls_shift/esd_max         0.368
_refine_ls_shift/esd_mean        0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2541
_refine_ls_wR_factor_obs         0.1676
_reflns_number_observed          1418
_reflns_number_total             2930
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907258f.txt
_cod_data_source_block           sn331/lc65
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7008945