Homoleptic phenolate complexes of zirconium(iv): syntheses and structural characterization of the first six coordinate complexes
Rosen, Thomas C.; Kirschbaum, Kristin; Giolando, Dean M.; Dalton Transactions  (2003) 120–; doi:10.1039/b207299h

data_7031185
_publ_section_title
;
 Homoleptic phenolate complexes of zirconium(iv): syntheses and structural
 characterization of the first six coordinate complexes
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              120
_journal_paper_doi               10.1039/b207299h
_journal_year                    2003
_chemical_formula_sum            'C48 H56 Cl6 N2 O8 Zr'
_chemical_formula_weight         1092.87
_chemical_name_systematic
; 
? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.604(2)
_cell_length_b                   13.538(3)
_cell_length_c                   18.379(4)
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.80
_cell_volume                     2616.3(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 and the Toledo cifomatic'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(1)
_diffrn_measured_fraction_theta_full 0.650
_diffrn_measured_fraction_theta_max 0.650
_diffrn_measurement_device_type  'CCD detector Smart platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17047
_diffrn_reflns_theta_full        33.04
_diffrn_reflns_theta_max         33.04
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.991136
_exptl_absorpt_correction_T_min  0.796622
_exptl_absorpt_correction_type
'Empirical :Multipole Expansion (Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_F_000             1128
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.3497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                4627
_reflns_number_total             6438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207299h.txt
_cod_data_source_block           '[NH2(CH3)2]2[Zr(OC6H4-2-Cl)6].2THF'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2616.3(9)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7031185