Synthesis, Structure, and Reactivity of Zirconium and Hafnium Imido Metalloporphyrins
Joseph L. Thorman; Ilia A. Guzei; Victor G. Young; L. Keith Woo; Inorganic Chemistry 38 (1999) 3814–3824; doi:10.1021/ic981399j

data_4322201
_publ_contact_author_address
;
   Department of Chemistry
   Iowa State University of Science and Technology
   Ames, Iowa, 50011
   USA
;
_publ_contact_author_email       iguzei@iastate.edu
_publ_contact_author_fax         +515-294-5717
_publ_contact_author_name
;
Ilia A. Guzei
;
_publ_contact_author_phone       +515-294-6419
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Zirconium and Hafnium Imido
 Metalloporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3814
_journal_page_last               3824
_journal_paper_doi               10.1021/ic981399j
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'J. Thorman / Prof. K. Woo - ISU'
_chemical_formula_sum            'C70.5 H69 N5 Zr'
_chemical_formula_weight         1077.53
_chemical_name_common            98061
_chemical_name_systematic
; 
 ? 
;
_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                 103.970(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6358(2)
_cell_length_b                   18.7583(1)
_cell_length_c                   19.4375(2)
_cell_measurement_temperature    173(2)
_cell_volume                     5886.24(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29098
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       Block
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.977
_refine_ls_goodness_of_fit_obs   1.029
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_restrained_S_obs      1.029
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_obs          0.0403
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.8549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1093
_refine_ls_wR_factor_obs         0.0984
_reflns_number_observed          7872
_reflns_number_total             10237
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981399j_1.cif
_cod_data_source_block           98061
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.8549P] 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^)+(0.0610P)^2^+1.8549P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C70.50 H69 N5 Zr'
_cod_database_code               4322201