Structures of [Co(II)(L)(NO3)(HOCH3)n]BPh4 (n = 4, 5) complexes (L = cis,cis-1,3,5-triaminocyclohexane-based ligand): structural ‘snapshots’ of anion binding to a metal centre
Boxwell, Clive J.; Walton, Paul H.; Chemical Communications  (1999) 1647–; doi:10.1039/a904802b

data_7110627
_publ_contact_author
;
Paul H. Walton
Department of Chemistry, University of York, Heslington, York, YO1 5DD, UK
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_publ_section_title
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 Structures of [Co(II)(L)(NO3)(HOCH3)n]BPh4 (n = 4, 5) complexes (L =
 cis,cis-1,3,5-triaminocyclohexane-based ligand): structural
 &#x2018;snapshots&#x2019; of anion binding to a metal centre
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1647
_journal_paper_doi               10.1039/a904802b
_journal_year                    1999
_chemical_formula_sum            'C75 H97 B Cl4 Co N4 O7'
_chemical_formula_weight         1378.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.21(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.393(4)
_cell_length_b                   16.811(5)
_cell_length_c                   21.737(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      11.09
_cell_measurement_theta_min      9.22
_cell_volume                     3768(2)
_computing_cell_refinement       teXsan
_computing_data_collection       teXsan
_computing_data_reduction        teXsan
_computing_molecular_graphics    teXsan
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  AFC6S
_diffrn_measurement_method       /w--2/q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_av_sigmaI/netI    0.1710
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5138
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        -1.257
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1932
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+5.3182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.2319
_reflns_number_gt                2322
_reflns_number_total             5138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904802bsup1.cif
_cod_data_source_block           shelxl2
_cod_depositor_comments
;
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 2 1'
_cod_database_code               7110627