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_4322204
_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_formula_sum            'C80 H77 N6 O Zr'
_chemical_formula_weight         1229.70
_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                97.1370(10)
_cell_angle_beta                 105.1960(10)
_cell_angle_gamma                100.5320(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9237(8)
_cell_length_b                   16.3912(10)
_cell_length_c                   16.6590(10)
_cell_measurement_temperature    173(2)
_cell_volume                     3292.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Vruker CCD-1000'
_diffrn_measurement_method       omega
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15220
_diffrn_reflns_theta_full        23.35
_diffrn_reflns_theta_max         23.35
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.218
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         9395
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                6933
_reflns_number_total             9395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981399j_4.cif
_cod_data_source_block           woo01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_database_code               4322204