μ-Peroxo-bis[<i>trans</i>-chloro(1,4,8,11-tetraazacyclotetradecane)cobalt(III)] bis(tetraphenylborate) diacetone solvate
Lewis, Gareth R.; Wilson, Claire; Acta Crystallographica Section C 57 (2001) 1159–1161; doi:10.1107/S0108270101012173

data_2012269
_publ_section_title
;\m-Peroxo-bis[<i>trans</i>-chloro(1,4,8,11-tetraazacyclotetradecane)cobalt(III)]
 bis(tetraphenylborate) diacetone solvate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1159
_journal_page_last               1161
_journal_paper_doi               10.1107/S0108270101012173
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac
'[Co2 Cl2 (O2) (C10 H24 N4)2] (C24 H20 B)2, 2C3 H6 O'
_chemical_formula_moiety
'C20 H48 Cl2 Co2 N8 O2 2+, 2C24 H20 B 1-, 2C3 H6 O'
_chemical_formula_sum            'C74 H100 B2 Cl2 Co2 N8 O4'
_chemical_formula_weight         1374.36
_chemical_name_systematic
;
\m~2~-Peroxo-bis[trans-chloro(1,4,8,11-tetraazacyclotetradecane)cobalt(III)]
bis(tetraphenylborate) diacetone solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 92.610(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.293(2)
_cell_length_b                   12.5644(13)
_cell_length_c                   18.225(2)
_cell_measurement_reflns_used    2759
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.35
_cell_volume                     3498.3(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT and SHELXTL (Sheldrick, 1997a)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max .904
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .041
_diffrn_reflns_av_sigmaI/netI    .047
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24509
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    .605
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .16
_refine_diff_density_max         .76
_refine_diff_density_min         -.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         8132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          .0825
_refine_ls_R_factor_gt           .0474
_refine_ls_shift/su_max          .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0590P)^2^+3.2407P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1336
_reflns_number_gt                5620
_reflns_number_total             8132
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            gg1072.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' 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:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
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_original_cell_volume        3498.2(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2012269
_cod_database_fobs_code          2012269