Tri-, deca- and dodecanuclear Co(iii)–pyrazolate metallacycles
Miras, Haralampos N.; Chakraborty, Indranil; Raptis, Raphael G.; Chemical Communications 46 (2010) 2569–; doi:10.1039/b920486e

data_7105387
_publ_section_title
;
 Tri-, deca- and dodecanuclear Co(iii)--pyrazolate metallacycles
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              2569
_journal_paper_doi               10.1039/b920486e
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C176 H198 Co12 N64 O43 P4'
_chemical_formula_weight         4729.02
_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           SHELXL-97
_cell_angle_alpha                83.77(3)
_cell_angle_beta                 86.82(3)
_cell_angle_gamma                70.93(3)
_cell_formula_units_Z            2
_cell_length_a                   18.694(4)
_cell_length_b                   19.172(4)
_cell_length_c                   35.964(7)
_cell_measurement_reflns_used    20927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5976
_cell_measurement_theta_min      3.1858
_cell_volume                     12107(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device_type  'Oxford Gemini Kappa CCD'
_diffrn_measurement_method       '\w & \p scans'
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.1711
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            105317
_diffrn_reflns_theta_full        28.66
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.8838
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4860
_exptl_crystal_size_max          0.4082
_exptl_crystal_size_mid          0.3092
_exptl_crystal_size_min          0.1448
_platon_squeeze_details
;
;
_refine_diff_density_max         3.412
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2418
_refine_ls_number_reflns         52366
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      2.122
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.1013
_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^)+(0.1812P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2934
_refine_ls_wR_factor_ref         0.3168
_reflns_number_gt                22613
_reflns_number_total             52366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920486e.txt
_cod_data_source_block           co12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        12108(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105387