Crystal structure of chlorido{[3-(η5-cyclopenta-dienyl)-2,2,3-trimethyl-1-phenylbutylidene] azanido-κN}[η2(N,O)-N,N-dimethylhydroxylaminato]titanium(IV), C20H27ClN2OTi
Večeřa, Miloš; Gyepes, Róbert; Lamač, Martin; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 457–459; doi:10.1515/ncrs-2016-0316

data_8106568
_publ_section_title
;
 Crystal structure of
 chlorido{[3-(\h5-cyclopenta-dienyl)-2,2,3-trimethyl-1-phenylbutylidene]
 azanido-\kN}[\h2(N,O)-N,N-dimethylhydroxylaminato]titanium(IV),
 C20H27ClN2OTi
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              457
_journal_page_last               459
_journal_paper_doi               10.1515/ncrs-2016-0316
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C20 H27 Cl N2 O Ti'
_chemical_formula_sum            'C20 H27 Cl N2 O Ti'
_chemical_formula_weight         394.78
_chemical_name_systematic
;
chlorido{[3-(\h^5^-cyclopentadienyl)-2,2,3-trimethyl-1-phenylbutylidene]\
azanido-\k<i>N</i>}[\h^2^(<i>N,O</i>)-<i>N,N</i>-dimethylhydroxylaminato]\
titanium(IV)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 97.9410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4006(2)
_cell_length_b                   10.8185(3)
_cell_length_c                   19.4821(5)
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      29.8279
_cell_measurement_theta_min      4.8532
_cell_volume                     1962.34(9)
_computing_cell_refinement       'SAINT [12]'
_computing_data_collection       'APEX2 [11]'
_computing_data_reduction        'SAINT [12]'
_computing_molecular_graphics    'PLATON [3]'
_computing_publication_material  'PLATON [3]'
_computing_structure_refinement  'SHELXL-2014/7 [2]'
_computing_structure_solution    'SHELXS-97 [2]'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31967
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 [10]'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.759
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.0657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4047
_reflns_number_total             4511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0316_suppl.cif
_cod_data_source_block           mv10_3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8106568
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              2533
_shelx_hkl_checksum              50118
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n