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_4516071
_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         'C14 H19 Cl O Ti'
_chemical_formula_sum            'C14 H19 Cl O Ti'
_chemical_formula_weight         286.64
_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             2016-05-24
_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                   15.01162(13)
_cell_length_b                   11.84446(11)
_cell_length_c                   15.51368(15)
_cell_measurement_reflns_used    10205
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.3530
_cell_measurement_theta_min      4.1340
_cell_volume                     2758.40(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -54.00  31.00   1.00    1.50    --  -37.14  38.00-120.00   85
  2  \w   -107.00  32.00   1.00    1.50    --  -37.14   0.00  30.00  139
  3  \w     22.00 103.00   1.00    1.50    --   37.14  57.00 -60.00   81
  4  \w     76.00 178.00   1.00    6.00    --  108.59  15.00  30.00  102
  5  \w     83.00 175.00   1.00    6.00    --  108.59  77.00-180.00   92
  6  \w     42.00 134.00   1.00    6.00    --  108.59 -77.00  60.00   92
  7  \w     92.00 174.00   1.00    6.00    --  108.59  61.00  90.00   82
  8  \w     83.00 175.00   1.00    6.00    --  108.59  77.00 -60.00   92
  9  \w     83.00 175.00   1.00    6.00    --  108.59  77.00 -90.00   92
 10  \w   -104.00 -12.00   1.00    1.50    --  -37.14 -77.00   0.00   92
 11  \w    -54.00  31.00   1.00    1.50    --  -37.14  38.00  90.00   85
 12  \w     17.00 102.00   1.00    1.50    --   37.14  67.00-158.00   85
 13  \w     93.00 176.00   1.00    6.00    --  108.59  45.00 150.00   83
 14  \w     93.00 157.00   1.00    6.00    --  108.59  45.00-120.00   64
;
_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      -0.0783208000
_diffrn_orient_matrix_UB_12      0.0450412000
_diffrn_orient_matrix_UB_13      -0.0541738000
_diffrn_orient_matrix_UB_21      -0.0017504000
_diffrn_orient_matrix_UB_22      0.1082754000
_diffrn_orient_matrix_UB_23      0.0549336000
_diffrn_orient_matrix_UB_31      0.0662928000
_diffrn_orient_matrix_UB_32      0.0561030000
_diffrn_orient_matrix_UB_33      -0.0625997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15770
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.527
_diffrn_reflns_theta_min         5.547
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.878
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0300P)^2^+1.2650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2638
_reflns_number_total             2724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cp2TiCl(OtBu).cif
_cod_data_source_block           nb02
_cod_database_code               4516071
_chemical_oxdiff_formula         C14H19Cl1O1Ti1
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C3(H3), C9(H9), C5(H5), C10(H10), C8(H8), C6(H6), C4(H4),
 C1(H1)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              91770
_shelx_hkl_checksum              63631
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-24
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_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 1.250
_oxdiff_exptl_absorpt_empirical_full_min 0.822