Insights into crystallization mechanism: a synchrotron study of polymorphism in a cobalt acetate cluster compound
Jonathan C. Burley; Timothy J. Prior; Acta Crystallographica Section C 62 (2006) m63–m66; doi:10.1107/S0108270105041570

data_2014323
_publ_section_title
;
 Insights into crystallization mechanism: a synchrotron study of
 polymorphism in a cobalt acetate cluster compound
;
_journal_coeditor_code           FA1176
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m63
_journal_page_last               m66
_journal_paper_doi               10.1107/S0108270105041570
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co3 (C2 H3 O2)4 (C5 H5 N)8] (P F6)2'
_chemical_formula_moiety         'C48 H52 Co3 N8 O8 2+ , 2F6 P -'
_chemical_formula_sum            'C48 H52 Co3 F12 N8 O8 P2'
_chemical_formula_weight         1335.71
_chemical_name_systematic
;
di-\m~3~-acetato-1\k^2^O,O':2\kO';2\kO:3\k^2^O,O'-di-\m~2~-acetato-
1\kO:2\kO';2\kO:3\kO'-octapyridyl-1\k^3^N,2\k^2^N,3\k^3^N-tricobalt(II)
bis(hexafluorophosphate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                99.3800(10)
_cell_angle_beta                 95.0080(10)
_cell_angle_gamma                92.2380(10)
_cell_formula_units_Z            4
_cell_length_a                   10.7354(6)
_cell_length_b                   22.1257(12)
_cell_length_c                   23.6103(13)
_cell_measurement_reflns_used    38731
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.64
_cell_measurement_theta_min      3.60
_cell_volume                     5503.9(5)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics
'WinGX (Version 1.64; Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_publication_material  SHEXLX97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 16.2SMX'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.84610
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38731
_diffrn_reflns_theta_full        31.64
_diffrn_reflns_theta_max         31.64
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1432
_refine_ls_number_reflns         21108
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0871P)^2^+8.495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                17966
_reflns_number_total             21108
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1176.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2014323
_cod_database_fobs_code          2014323