Synthesis of Zirconium Aryloxide Complexes Containing Pendent Vinyl Groups
William J. Evans; Mohammad A. Ansari; Joseph W. Ziller; Inorganic Chemistry 38 (1999) 1160–1164; doi:10.1021/ic981201v

data_4321850
_publ_section_title
;
 Synthesis of Zirconium Aryloxide Complexes Containing Pendent Vinyl
 Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1160
_journal_page_last               1164
_journal_paper_doi               10.1021/ic981201v
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C100 H130 K4 O23 Zr2'
_chemical_formula_weight         2038.88
_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           SHELXTL
_cell_angle_alpha                82.06
_cell_angle_beta                 65.46
_cell_angle_gamma                67.51
_cell_formula_units_Z            1
_cell_length_a                   13.933(3)
_cell_length_b                   14.451(4)
_cell_length_c                   15.924(4)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    158
_cell_measurement_theta_max      11.37
_cell_measurement_theta_min      6.31
_cell_volume                     2694.0(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        CARESS
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      158
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         rotating-anode
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7384
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.807
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_obs          0.0901
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1799P)^2^+16.1291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2776
_refine_ls_wR_factor_obs         0.2570
_reflns_number_observed          5855
_reflns_number_total             7033
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981201v_3.cif
_cod_data_source_block           maa30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.1799P)^2^+16.1291P] 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^)+(0.1799P)^2^+16.1291P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321850