Polymorphs of [(2<i>S</i>,3<i>S</i>)-α-Me-<i>N</i>,<i>N</i>'-bis(salicylidene)butane-2,3-diaminato]bis(pyridine)cobalt(III) tetrafluoroborate hydrate
Shoichi Sato; Takashi Fukuda; Kazuaki Ishii; Yoshiharu Nakano; Yuki Fujii; Acta Crystallographica Section C 55 (1999) 1466–1470; doi:10.1107/S0108270199006812

data_2008875
_publ_section_title
;Polymorphs of
 [(2<i>S</i>,3<i>S</i>)-\a-Me-<i>N</i>,<i>N</i>'-bis(salicylidene)butane-2,3-diaminato]bis(pyridine)cobalt(III)
 tetrafluoroborate hydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1466
_journal_page_last               1470
_journal_paper_doi               10.1107/S0108270199006812
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac
'[Co (C20 H22 N2 O2) (C5 H5 N)2] (B F4), 1.5H2 O'
_chemical_formula_moiety         'C30 H35 Co1 N4 O3.5 B1 F4'
_chemical_formula_sum            'C30 H35 B Co F4 N4 O3.5'
_chemical_formula_weight         653.2
_chemical_name_systematic
'[Co{\a-Me--sal~2~--(S,S)--bn}(py)~2~}]BF~4~, 1.5-water'
_space_group_IT_number           179
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   10.422(6)
_cell_length_b                   10.422(6)
_cell_length_c                   101.433(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      25.9
_cell_volume                     9541(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection
'MSC/AFC Diffractometer Control (Rigaku Corporation, 1991)'
_computing_data_reduction
'TEXSAN  (Molecular Structure Corporation, 1995)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'DIRDIF92 (PATTY) (Beurskens et al., 1992)'
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.079
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       125
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13193
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        62.5
_diffrn_reflns_theta_max         72.5
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        3.16
_diffrn_standards_interval_count 150
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    4.77
_exptl_absorpt_correction_T_max  0.298
_exptl_absorpt_correction_T_min  0.170
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(De Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             4066.8
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.13
_refine_ls_abs_structure_details 'see text'
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.892
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     390
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00027|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                3903
_reflns_number_total             6299
_reflns_threshold_expression     I>1.5\s(I)
_cod_data_source_file            cf1272.cif
_cod_data_source_block           hexagonal
_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_cell_volume        9541.(8)
_cod_original_formula_sum        'C30 H35 B1 Co1 F4 N4 O3.5'
_cod_database_code               2008875