Synthesis and characterization of a <i>tert-</i>butyl ester-substituted titanocene dichloride: ^<i>t^-BuOOC</i>Cp~2~TiCl~2~
McCarthy, Jackson S.; McMillen, Colin D.; Pienkos, Jared A.; Wagenknecht, Paul S.; Acta Crystallographica Section E 76 (2020) 1562–1565; doi:10.1107/S2056989020011834

data_2243589
_publ_section_title
;
 Synthesis and characterization of a <i>tert-</i>butyl ester-substituted
 titanocene dichloride: ^<i>t^-BuOOC</i>Cp~2~TiCl~2~
;
_journal_coeditor_code           PK2643
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1562
_journal_page_last               1565
_journal_paper_doi               10.1107/S2056989020011834
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ti (C10 H13 O2)2 Cl2]'
_chemical_formula_moiety         'C20 H26 Cl2 O4 Ti'
_chemical_formula_sum            'C20 H26 Cl2 O4 Ti'
_chemical_formula_weight         449.21
_chemical_name_systematic
;
Bis[\h^5^-(<i>tert</i>-butoxycarbonyl)cyclopentadienyl]dichloridotitanium(IV)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 91.214(3)
_cell_angle_gamma                90
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_cell_length_a                   29.3802(19)
_cell_length_b                   10.8106(7)
_cell_length_c                   13.6002(9)
_cell_measurement_reflns_used    8394
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.50
_cell_volume                     4318.7(5)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2016 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18758
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.007
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       column
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0482
_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^)+22.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                3053
_reflns_number_total             4007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2643sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243589
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.975
_shelx_hkl_checksum              87648
_shelx_res_checksum              11160
_cod_database_fobs_code 2243589