Syntheses and characterization of mixed acetylacetonate‒catecholate complexes of zirconium, [Zr3(acac)4(cat)4(MeOH)2], [Zr(acac)2(DBcat)]2 (H2DBcat = 3,5-di-tert-butylcatechol) and [Zr4(μ4-O)(acac)4(DBcat)3(OMe)4(MeOH)]
Chi, Yun; Lan, Jing-Wen; Ching, Wei-Li; Peng, Shie-Ming; Lee, Gene-Hsiang; Journal of the Chemical Society, Dalton Transactions  (2000) 2923–; doi:10.1039/b002705g

data_7009688
_publ_section_title
;
 Syntheses and characterization of mixed acetylacetonate--catecholate
 complexes of zirconium, [Zr3(acac)4(cat)4(MeOH)2], [Zr(acac)2(DBcat)]2
 (H2DBcat&#x2005;=&#x2005;3,5-di-tert-butylcatechol) and
 [Zr4(\m4-O)(acac)4(DBcat)3(OMe)4(MeOH)]
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2923
_journal_paper_doi               10.1039/b002705g
_journal_year                    2000
_chemical_formula_moiety         'C73 H118 O23 Cl6 Zr4 '
_chemical_formula_sum            'C73 H118 Cl6 O23 Zr4'
_chemical_formula_weight         1941.30
_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'
_cell_angle_alpha                75.947(20)
_cell_angle_beta                 85.394(20)
_cell_angle_gamma                82.520(19)
_cell_formula_units_Z            2
_cell_length_a                   13.234(3)
_cell_length_b                   14.387(3)
_cell_length_c                   25.277(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      12.81
_cell_measurement_theta_min      7.55
_cell_volume                     4623.0(17)
_computing_cell_refinement       CAD4-express
_computing_data_collection       CAD4-express
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    'NRCVAX ORTEP'
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Theta/2theta scan b/P/b '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.010
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16301
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.67
_exptl_absorpt_correction_T_max  0.8060
_exptl_absorpt_correction_T_min  0.7467
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             1982.57
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.65
_refine_ls_extinction_coef       3068(82)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   1.27
_refine_ls_matrix_type           atomblock
_refine_ls_number_parameters     965
_refine_ls_number_reflns         10349
_refine_ls_R_factor_all          0.090
_refine_ls_R_factor_obs          0.049
_refine_ls_shift/esd_max         0.014
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_all         0.086
_refine_ls_wR_factor_obs         0.052
_reflns_number_observed          10349
_reflns_number_total             16228
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            b002705g.txt
_cod_data_source_block           ic6050
_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        4623.0(16)
_cod_original_formula_sum        'C73 H118 O23 Cl6 Zr4 '
_cod_database_code               7009688