Homoleptic phenolate complexes of zirconium(iv): syntheses and structural characterization of the first six coordinate complexes
Rosen, Thomas C.; Kirschbaum, Kristin; Giolando, Dean M.; Dalton Transactions  (2003) 120–; doi:10.1039/b207299h

data_7031184
_publ_section_title
;
 Homoleptic phenolate complexes of zirconium(iv): syntheses and structural
 characterization of the first six coordinate complexes
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              120
_journal_paper_doi               10.1039/b207299h
_journal_year                    2003
_chemical_formula_sum            'C52 H56 Cl6 Na2 O10 Zr'
_chemical_formula_weight         1190.87
_chemical_name_systematic
; 
? 
;
_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                111.212(1)
_cell_angle_beta                 109.659(1)
_cell_angle_gamma                96.699(1)
_cell_formula_units_Z            1
_cell_length_a                   10.8102(2)
_cell_length_b                   12.1126(3)
_cell_length_c                   12.2598(2)
_cell_measurement_reflns_used    7940
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.88
_cell_measurement_theta_min      2.69
_cell_volume                     1356.35(5)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL and the Toledo cifomatic'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'CCD detector Smart Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16012
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.991925
_exptl_absorpt_correction_T_min  0.854298
_exptl_absorpt_correction_type
'Empirical :Multipole Expansion (Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         7139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.2280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                5771
_reflns_number_total             7139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207299h.txt
_cod_data_source_block           '[Na(THF)2]2[Zr(OC6H4-2-Cl)6]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7031184