X-Ray structure and solvolytic activity towards phosphate diesters of a zirconium(IV) complex
Stulz, Eugen; Leumann, Christian; Chemical Communications  (1999) 239–; doi:10.1039/a809101c

data_7110416
_publ_section_title
;
 X-Ray structure and solvolytic activity towards phosphate diesters of a
 zirconium(IV) complex
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              239
_journal_paper_doi               10.1039/a809101c
_journal_year                    1999
_chemical_formula_sum            'C38 H46 N2 O12 Zr2'
_chemical_formula_weight         905.21
_chemical_name_common            Zr(IV)(acac)2sae
_chemical_name_systematic
;
 bis-(acetylacetonato)-N(2-hydroxyethyl)salicylidenimino-zirconium(IV)
;
_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                89.32(3)
_cell_angle_beta                 70.01(3)
_cell_angle_gamma                86.67(3)
_cell_formula_units_Z            2
_cell_length_a                   11.642(2)
_cell_length_b                   12.002(2)
_cell_length_c                   15.718(3)
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.18
_cell_volume                     2060.4(7)
_computing_cell_refinement       'CELL (Stoe & Cie Gmbh, Darmstadt, 1996)'
_computing_data_collection       'EXPOSE (Stoe & Cie Gmbh, Darmstadt, 1996)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie Gmbh, Darmstadt, 1996)'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'STOE Image Plate Diffraction system'
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.1133
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16331
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.2mm
_exptl_crystal_size_mid          0.2mm
_exptl_crystal_size_min          0.2mm
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                4338
_reflns_number_total             7494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            809101csup1.cif
_cod_data_source_block           zr5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'triclin' was replaced with
'triclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0640P)^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^)+(0.0640P)^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_sg_symbol_H-M      P-1
_cod_database_code               7110416