Multicomponent Mechanochemical Synthesis of Cyclopentadienyl Titanium <i>tert</i>-Butoxy Halides, Cp <sub> <i>x</i> </sub> TiX <sub> <i>y</i> </sub> (O <sup> <i>t</i> </sup> Bu)<sub>4-(<i>x</i>+<i>y</i>)</sub> (<i>x</i>, <i>y</i> = 1, 2; X = Cl, Br).
Boyde, Nicholas C.; Steelman, Grant W.; Hanusa, Timothy P.; ACS omega 3 (2018) 8149–8159; doi:10.1021/acsomega.8b00943

data_4516073
_publ_section_title
;
 Multicomponent Mechanochemical Synthesis of Cyclopentadienyl Titanium
 <i>tert</i>-Butoxy Halides, Cp <sub> <i>x</i> </sub> TiX <sub> <i>y</i>
 </sub> (O <sup> <i>t</i> </sup> Bu)<sub>4-(<i>x</i>+<i>y</i>)</sub>
 (<i>x</i>, <i>y</i> = 1, 2; X = Cl, Br).
;
_journal_issue                   7
_journal_name_full               'ACS omega'
_journal_page_first              8149
_journal_page_last               8159
_journal_paper_doi               10.1021/acsomega.8b00943
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C10.91 H12.73 Cl1.09 O0.91 Ti'
_chemical_formula_sum            'C10.91 H12.73 Cl1.09 O0.91 Ti'
_chemical_formula_weight         244.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4890(3)
_cell_length_b                   11.4556(2)
_cell_length_c                   14.6289(3)
_cell_measurement_reflns_used    8781
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.4410
_cell_measurement_theta_min      3.5490
_cell_volume                     2092.94(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43g (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -2.00  92.00   1.00    8.49    --   24.36  77.00-150.00   94
  2  \w     -2.00  92.00   1.00    8.49    --   24.36  77.00  90.00   94
  3  \w     -2.00  92.00   1.00    8.49    --   24.36  77.00 -60.00   94
  4  \w    -43.00  10.00   1.00    8.49    --   24.36 -77.00-180.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0197133000
_diffrn_orient_matrix_UB_12      0.0229464000
_diffrn_orient_matrix_UB_13      0.0417593000
_diffrn_orient_matrix_UB_21      -0.0200728000
_diffrn_orient_matrix_UB_22      -0.0495010000
_diffrn_orient_matrix_UB_23      0.0235331000
_diffrn_orient_matrix_UB_31      0.0493643000
_diffrn_orient_matrix_UB_32      -0.0292975000
_diffrn_orient_matrix_UB_33      -0.0070942000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17721
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.729
_diffrn_reflns_theta_min         3.228
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43g (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3612
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3213
_reflns_number_total             3612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cp2TiCl(OMe).cif
_cod_data_source_block           nb08
_cod_original_cell_volume        2092.94(7)
_cod_database_code               4516073
_chemical_oxdiff_formula         C11H13OTiCl
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2A-Ti1 \\sim Ti1-Cl1
 with sigma of 0.02
3. Others
 Sof(Cl2A)=1-FVAR(1)
 Sof(O1)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10)
4.b Idealised Me refined as rotating group:
 C11(H11B,H11C,H11A)
;
_shelx_res_checksum              43006
_shelx_hkl_checksum              38853
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-12
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.201
_oxdiff_exptl_absorpt_empirical_full_min 0.743