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_4303982
_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_sum            'C47 H39 Cl3 Hf N4 O7 S'
_chemical_formula_weight         1088.72
_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                66.15(3)
_cell_angle_beta                 86.36(3)
_cell_angle_gamma                67.92(3)
_cell_formula_units_Z            2
_cell_length_a                   11.951(2)
_cell_length_b                   14.653(3)
_cell_length_c                   14.865(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2194.2(11)
_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 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23739
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    2.665
_exptl_absorpt_correction_T_max  0.7765
_exptl_absorpt_correction_T_min  0.4153
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.662
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+11.9928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                8976
_reflns_number_total             9648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700840j-file008.cif
_cod_data_source_block           x1588l
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        2194.2(12)
_cod_database_code               4303982