Catechol derivatives of Group 4 and 5 compounds
Timothy J. Boyle; Louis J. Tribby; Todd M. Alam; Scott D. Bunge; Gregory P. Holland; Polyhedron 24 (2005) 1143–1152; doi:10.1016/j.poly.2005.03.055

data_1512902
_publ_section_title
;
 Catechol derivatives of Group 4 and 5 compounds
;
_journal_issue                   10
_journal_name_full               Polyhedron
_journal_page_first              1143
_journal_page_last               1152
_journal_paper_doi               10.1016/j.poly.2005.03.055
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C68 H52 Hf4 N4 O17'
_chemical_formula_weight         1911.10
_chemical_name_common            '(3) Hf4(O)(cat)6(cat-H)2(py)4'
_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                 100.058(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.960(8)
_cell_length_b                   15.372(5)
_cell_length_c                   27.916(10)
_cell_measurement_reflns_used    881
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      20.70
_cell_measurement_theta_min      2.59
_cell_volume                     9701(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1025
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51713
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.315
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         11.506
_refine_diff_density_min         -3.209
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1458
_refine_ls_R_factor_gt           0.1120
_refine_ls_shift/su_max          3.063
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1832P)^2^+312.6223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2854
_refine_ls_wR_factor_ref         0.3038
_reflns_number_gt                9819
_reflns_number_total             13781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2005-1143.cif
_cod_data_source_block           c:\frames\jan161_hfcat\workold\jan162ss
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512902