Routes to New Hafnium(IV) Tetraaryl Porphyrins and Crystal Structures of Unusual Phosphate-, Sulfate-, and Peroxide-Bridged Dimers
Alexander Falber; Louis Todaro; Israel Goldberg; Michael V. Favilla; Charles Michael Drain; Inorganic Chemistry 47 (2008) 454–467; doi:10.1021/ic700840j

data_4303983
_publ_section_title
;
Routes to New Hafnium(IV) Tetraaryl Porphyrins and Crystal Structures of
Unusual Phosphate-, Sulfate-, and Peroxide-Bridged Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              454
_journal_page_last               467
_journal_paper_doi               10.1021/ic700840j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C49 H40 Hf N4 O5 S, 1.5(C Cl3)'
_chemical_formula_sum            'C50.5 H40 Cl4.5 Hf N4 O5 S'
_chemical_formula_weight         1152.94
_chemical_name_systematic
;
 ?
;
_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                 91.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.624(3)
_cell_length_b                   21.489(4)
_cell_length_c                   15.044(3)
_cell_measurement_temperature    100(2)
_cell_volume                     4726.3(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1540
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            67862
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    2.558
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.7321
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2302
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         8292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+44.8717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                5817
_reflns_number_total             8292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700840j-file009.cif
_cod_data_source_block           x1580l
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_formula_sum        'C50.50 H40 Cl4.50 Hf N4 O5 S'
_cod_database_code               4303983