Zirconium mixed ligand isopropoxide/aminoalkoxide complexes: crystal structures of [Zr2(OPri)6(L)2] and [Zr2(OBut)3(bdmap)4(OH)] {where L = dmap, 1-dimethylaminopropan-2-olate and bdmap, 1,1-bis(dimethylamino)propan-2-olate}
Fleeting, Kirsty A.; O’Brien, Paul; Jones, Anthony C.; Otway, David J.; White, Andrew J. P.; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (1999) 2853–; doi:10.1039/a901666j

data_7027344
_publ_section_title
;
 Zirconium mixed ligand isopropoxide/aminoalkoxide complexes: crystal
 structures of [Zr2(OPri)6(L)2] and [Zr2(OBut)3(bdmap)4(OH)] {where
 L&#x2005;=&#x2005;dmap, 1-dimethylaminopropan-2-olate and bdmap,
 1,1-bis(dimethylamino)propan-2-olate}
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2853
_journal_paper_doi               10.1039/a901666j
_journal_year                    1999
_chemical_formula_sum            'C40 H96 N8 O8 Zr2'
_chemical_formula_weight         999.69
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.494(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.949(2)
_cell_length_b                   12.276(2)
_cell_length_c                   23.485(3)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.55
_cell_measurement_theta_min      4.88
_cell_volume                     5619.6(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_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      203(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10156
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        10.22
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       'blocky plates'
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00028(7)
_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   1.032
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9871
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+1.7315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1083
_refine_ls_wR_factor_obs         0.0950
_reflns_number_observed          7323
_reflns_number_total             9871
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901666jsup1.cif
_cod_data_source_block           POB9706
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+1.7315P] 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^)+(0.0478P)^2^+1.7315P] 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        5619.5(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027344