Group IV Imino-Semiquinone Complexes Obtained by Oxidative Addition of Halogens
Karen J. Blackmore; Michael B. Sly; Mason R. Haneline; Joseph W. Ziller; Alan F. Heyduk; Inorganic Chemistry 47 (2008) 10522–10532; doi:10.1021/ic801127r

data_4306283
_publ_section_title
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Group IV Imino-Semiquinone Complexes Obtained by Oxidative Addition of
Halogens
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10522
_journal_page_last               10532
_journal_paper_doi               10.1021/ic801127r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C72 H116 N4 O4 Zr2'
_chemical_formula_weight         1284.13
_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           SHELXTL
_cell_angle_alpha                88.275(4)
_cell_angle_beta                 85.543(3)
_cell_angle_gamma                79.574(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5149(19)
_cell_length_b                   14.213(2)
_cell_length_c                   21.610(4)
_cell_measurement_temperature    163(2)
_cell_volume                     3467.3(10)
_computing_cell_refinement       'Bruker SMART/SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
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_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0890
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_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         0.95
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.9560
_exptl_absorpt_correction_T_min  0.9303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1964
_reflns_number_gt                6766
_reflns_number_total             11837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801127r_si_002_1.cif
_cod_data_source_block           afh77
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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        3467.4(10)
_cod_database_code               4306283