Crystal structure of 1,1-bis(η 5-adamantylcyclopentadienyl)-3-phenyl-2-trimethylsilyl-2,3-dihydroisotitanazole, C42H55NSiTi
Manßen, Manfred; Schmidtmann, Marc; Beckhaus, Rüdiger; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 671–673; doi:10.1515/ncrs-2016-0404

data_8106638
_publ_section_title
;
 Crystal structure of 1,1-bis(\h
 5-adamantylcyclopentadienyl)-3-phenyl-2-trimethylsilyl-2,3-dihydroisotitanazole,
 C42H55NSiTi
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              671
_journal_page_last               673
_journal_paper_doi               10.1515/ncrs-2016-0404
_journal_volume                  232
_journal_year                    2017
_chemical_formula_structural     Ti(C15H19)2(C9H8NSi(CH3)3)
_chemical_formula_sum            'C42 H55 N Si Ti'
_chemical_formula_weight         649.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                69.6151(13)
_cell_angle_beta                 85.3502(14)
_cell_angle_gamma                83.8861(14)
_cell_formula_units_Z            2
_cell_length_a                   9.2556(4)
_cell_length_b                   12.5048(5)
_cell_length_c                   15.7350(7)
_cell_measurement_reflns_used    8166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.99
_cell_measurement_theta_min      2.22
_cell_volume                     1695.51(13)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32114
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         1.382
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.968491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         32114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                28454
_reflns_number_total             32114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0404_suppl.cif
_cod_data_source_block           mmtw1_5
_cod_database_code               8106638
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              74790
_shelx_hkl_checksum              76625