Phenoxyl Radical Complexes of Zinc(II)
Achim Sokolowski; Jochen Müller; Thomas Weyhermüller; Robert Schnepf; Peter Hildebrandt; Knut Hildenbrand; Eberhard Bothe; Karl Wieghardt; Journal of the American Chemical Society 119 (1997) 8889–8900; doi:10.1021/ja970417d

data_4117028
_publ_section_title
;
 Phenoxyl Radical Complexes of Zinc(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8889
_journal_page_last               8900
_journal_paper_doi               10.1021/ja970417d
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C47.5 H69 N3 O3 Zn'
_chemical_formula_weight         795.43
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.23(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.118(2)
_cell_length_b                   19.723(3)
_cell_length_c                   19.266(3)
_cell_measurement_reflns_used    7384
_cell_measurement_temperature    100(2)
_cell_volume                     4463.4(13)
_computing_cell_refinement       'SAINT V4.05 Siemens'
_computing_data_collection       SMART
_computing_data_reduction        'SAINT V4.05 Siemens'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.1044
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34664
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.56
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_obs          0.0479
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+4.9569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1336
_refine_ls_wR_factor_obs         0.1206
_reflns_number_observed          6751
_reflns_number_total             7829
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja970417d_2.cif
_cod_data_source_block           2475
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+4.9569P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+4.9569P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4463.4(12)
_cod_original_formula_sum        'C47.50 H69 N3 O3 Zn'
_cod_database_code               4117028