High-Vacuum Pyrolysis of Zr(2,3,7,8,12,13,17,18-Octaethylporphyrin)(PhC\τbCPh) as a Route to Novel Zr Species: X-ray Structure of a Hetero-Triply Bridged Species, [(OEP)Zr(μ-Cl)]2(μ-O)
James P. Collman; Roman Boulatov; Geoffrey B. Jameson; Vipin Narang; Inorganic Chemistry 41 (2002) 416–420; doi:10.1021/ic0108078

data_4317430
_publ_contact_author_address
;
      Department of Chemistry
Stanford University
Stanford, CA 94305-5080
;
_publ_contact_author_email       ' jpc@stanford.edu '
_publ_contact_author_fax         ' 650-7250259 '
_publ_contact_author_name        ' Prof. James P. Collman'
_publ_contact_author_phone       ' 650 - 7250283 '
_publ_section_title
;
 High-Vacuum Pyrolysis of
 Zr(2,3,7,8,12,13,17,18-Octaethylporphyrin)(PhC\\tbCPh) as a Route to
 Novel Zr Species: X-ray Structure of a Hetero-Triply Bridged Species,
 [(OEP)Zr(\m-Cl)]2(\m-O)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              416
_journal_page_last               420
_journal_paper_doi               10.1021/ic0108078
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C72 H88 Cl2 N8 O Zr2'
_chemical_formula_weight         1334.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.016(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.836(4)
_cell_length_b                   15.084(4)
_cell_length_c                   23.170(5)
_cell_measurement_reflns_used    1261
_cell_measurement_temperature    177
_cell_measurement_theta_max      39.6
_cell_measurement_theta_min      3.65
_cell_volume                     6483(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5846
_diffrn_reflns_theta_full        19.78
_diffrn_reflns_theta_max         19.78
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.455
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          .007
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.712
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         5846
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      0.692
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.083
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                2434
_reflns_number_total             5846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0108078.cif
_cod_data_source_block           rb6
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4317430