Zirconium−Butadiene Bonded over a Planar Set of Oxygens Derived from Calix[4]arene and Its Behavior as a Source of Zirconium(II)
Caselli, Alessandro; Giannini, Luca; Solari, Euro; Floriani, Carlo; Re, Nazzareno; Chiesi-Villa, Angiola; Rizzoli, Corrado; Organometallics 16 (1997) 5457–; doi:10.1021/om970624m

data_4078346
_publ_section_title
;
 Zirconium&#x2212;Butadiene Bonded over a Planar Set of Oxygens Derived
 from Calix[4]arene and Its Behavior as a Source of Zirconium(II)
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5457
_journal_paper_doi               10.1021/om970624m
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C71 H87 N O4 Zr'
_chemical_formula_weight         1109.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 90.15(1)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   15.559(2)
_cell_length_b                   16.936(2)
_cell_length_c                   23.580(4)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    25
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      18.2
_cell_volume                     6213.5(15)
_computing_cell_refinement       'TEXSAN Software'
_computing_data_collection       'TEXSAN Software'
_computing_data_reduction        'TEXSAN Software'
_computing_structure_refinement  'SHELXS-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      143
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2158
_diffrn_reflns_av_sigmaI/netI    0.3230
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10140
_diffrn_reflns_theta_max         70.43
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.8076
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   'North et al. 1968'
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.1862
_exptl_crystal_description       irregular_prism
_exptl_crystal_F_000             2368.0
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.568
_refine_diff_density_min         -.904
_refine_diff_density_rms         .121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.238
_refine_ls_hydrogen_treatment    'not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         7317
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.227
_refine_ls_R_factor_all          0.3015
_refine_ls_R_factor_obs          0.0814
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2582
_refine_ls_wR_factor_obs         0.1971
_reflns_number_observed          3105
_reflns_number_total             9554
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om5457.cif
_cod_data_source_block           COMPLEX_14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.0000P] 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^)+(0.1282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6213.(2)
_cod_original_sg_symbol_H-M      'P 21/N              '
_cod_database_code               4078346