A new polymorph of <i>fac</i>-tris(4,6-dimethylpyrimidine-2-thiolato-κ^2^<i>N,S</i>)cobalt(III) monohydrate
Burrow, Robert Alan; Schulz Lang, Ernesto; Fernandes Jr, Ramão Marceli; Vázquez-López, Ezequiel M.; Acta Crystallographica Section E 59 (2003) m396–m398; doi:10.1107/S1600536803011486

data_2202837
_publ_section_title
;A new polymorph of
 <i>fac</i>-tris(4,6-dimethylpyrimidine-2-thiolato-\k^2^<i>N,S</i>)cobalt(III)
 monohydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m396
_journal_page_last               m398
_journal_paper_doi               10.1107/S1600536803011486
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Co (C6 H7 N2 S1)3], H2 O'
_chemical_formula_moiety         'C18 H21 Co N6 S3, H2 O'
_chemical_formula_sum            'C18 H23 Co N6 O S3'
_chemical_formula_weight         494.56
_chemical_name_systematic
;
fac-tris(4,6-dimethylpyrimidine-2-thiolato-N,S)cobalt(III) monohydrate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.969(2)
_cell_length_b                   8.0436(11)
_cell_length_c                   16.552(2)
_cell_measurement_reflns_used    3091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.7
_cell_measurement_theta_min      5.5
_cell_volume                     2259.2(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1026
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12629
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         2.4
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.8406
_exptl_absorpt_correction_T_min  0.8242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(DENZO-SMN, Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.332
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5124
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0482P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                2380
_reflns_number_total             5124
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6145.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2202837
_cod_database_fobs_code          2202837