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_7009686
_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_sum            'C50.5 H65 Cl5 O20 Zr3'
_chemical_formula_weight         1442.94
_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
_cell_angle_alpha                87.015(1)
_cell_angle_beta                 87.615(1)
_cell_angle_gamma                67.292(1)
_cell_formula_units_Z            2
_cell_length_a                   13.9458(2)
_cell_length_b                   14.1348(3)
_cell_length_c                   17.1990(3)
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    295(2)
_cell_volume                     3122.39(10)
_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'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37666
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        15
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.8313
_exptl_absorpt_correction_T_min  0.7170
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_obs          0.0447
_refine_ls_shift/esd_max         -2.466
_refine_ls_shift/esd_mean        0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+2.6260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1299
_refine_ls_wR_factor_obs         0.1147
_reflns_number_observed          9523
_reflns_number_total             12767
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002705g.txt
_cod_data_source_block           ic5599
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+2.6260P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+2.6260P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C50.50 H65 Cl5 O20 Zr3'
_cod_database_code               7009686