Five- and Six-Coordinate Group 4 Compounds Stabilized by β-Ketiminate and Diketiminate Ligands: Syntheses and Comparisons between Solid-State and Solution Structures
Lena Kakaliou; Scanlon; Baixin Qian; Sung W. Baek; Milton R. Smith; Douglas H. Motry; Inorganic Chemistry 38 (1999) 5964–5977; doi:10.1021/ic981364j

data_4322537
_publ_section_title
;
 Five- and Six-Coordinate Group 4 Compounds Stabilized by \b-Ketiminate
 and Diketiminate Ligands: Syntheses and Comparisons between Solid-State
 and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5964
_journal_page_last               5977
_journal_paper_doi               10.1021/ic981364j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C38 H42 Cl2 N4 Zr'
_chemical_formula_weight         716.88
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.179(2)
_cell_length_b                   22.868(5)
_cell_length_c                   16.813(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3487.9(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21485
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.501
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.019
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_obs          0.0348
_refine_ls_shift/esd_max         -0.311
_refine_ls_shift/esd_mean        0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.5970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0770
_refine_ls_wR_factor_obs         0.0706
_reflns_number_observed          6292
_reflns_number_total             8272
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_10.cif
_cod_data_source_block           (TTP)2ZrCl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.5970P] 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^)+(0.0351P)^2^+0.5970P] 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        3487.9(12)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4322537