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_4322531
_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            'C25 H39 N5 Zr'
_chemical_formula_weight         500.83
_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
_cell_angle_alpha                102.19(3)
_cell_angle_beta                 92.92(3)
_cell_angle_gamma                101.28(3)
_cell_formula_units_Z            2
_cell_length_a                   8.669(2)
_cell_length_b                   10.385(2)
_cell_length_c                   15.874(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1363.5(5)
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.5916
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11671
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.422
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.300
_refine_ls_goodness_of_fit_obs   0.549
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.300
_refine_ls_restrained_S_obs      0.549
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_obs          0.0575
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1527
_refine_ls_wR_factor_obs         0.1382
_reflns_number_observed          1525
_reflns_number_total             6153
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_04.cif
_cod_data_source_block           (TTP)Zr(NMe2)3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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_database_code               4322531