Reaction environment and ligand lability in group 4 Cp2MXY (X, Y = Cl, OtBu) complexes.
Boyde, Nicholas C.; Rightmire, Nicholas R.; Bierschenk, Eric J.; Steelman, Grant W.; Hanusa, Timothy P.; Brennessel, William W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18635–18642; doi:10.1039/c6dt03199d

data_7041078
_publ_section_title
;
 Reaction environment and ligand lability in group 4 Cp2MXY (X, Y = Cl,
 OtBu) complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18635
_journal_page_last               18642
_journal_paper_doi               10.1039/c6dt03199d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C19 H24 O Ti'
_chemical_formula_sum            'C19 H24 O Ti'
_chemical_formula_weight         316.28
_chemical_name_systematic        tris(cyclopentadienyl)titanium(tert-butoxide)
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-28 deposited with the CCDC.
2016-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4641(2)
_cell_length_b                   19.4641(2)
_cell_length_c                   8.58573(12)
_cell_measurement_reflns_used    8277
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.3200
_cell_measurement_theta_min      4.5100
_cell_volume                     3252.71(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      air
_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 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w   -106.00 -20.00   1.00    5.00    --  -37.14 -38.00 -30.00   86
  2  \w   -104.00 -12.00   1.00    5.00    --  -37.14 -77.00 -90.00   92
  3  \w     22.00 103.00   1.00    5.00    --   37.14  57.00-180.00   81
  4  \w     92.00 174.00   1.00   15.00    --  108.59  61.00 -60.00   82
  5  \w     40.00 128.00   1.00   15.00    --  108.59 -30.00 -90.00   88
  6  \w     44.00 125.00   1.00   15.00    --  108.59 -61.00-150.00   81
  7  \w     89.00 177.00   1.00   15.00    --  108.59  30.00  90.00   88
  8  \w    -52.00  29.00   1.00    5.00    --  -37.14  57.00 -60.00   81
  9  \w    -62.00  29.00   1.00    5.00    --  -37.14  77.00  90.00   91
 10  \w     92.00 174.00   1.00   15.00    --  108.59  61.00   0.00   82
 11  \w     42.00 132.00   1.00   15.00    --  108.59 -77.00  30.00   90
 12  \w     83.00 140.00   1.00   15.00    --  108.59  77.00-120.00   57
;
_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      0.0021874000
_diffrn_orient_matrix_UB_12      0.0676022000
_diffrn_orient_matrix_UB_13      0.0932326000
_diffrn_orient_matrix_UB_21      -0.0091671000
_diffrn_orient_matrix_UB_22      -0.0406275000
_diffrn_orient_matrix_UB_23      0.1525464000
_diffrn_orient_matrix_UB_31      0.0785934000
_diffrn_orient_matrix_UB_32      -0.0065714000
_diffrn_orient_matrix_UB_33      0.0152015000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.503
_diffrn_reflns_theta_min         3.211
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.409
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes'
_exptl_crystal_size_max          0.546
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0320P)^2^+1.1430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2798
_reflns_number_total             3189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03199d2.cif
_cod_data_source_block           nb01
_cod_depositor_comments
'Adding full bibliography for 7041078--7041081.cif.'
_cod_original_cell_volume        3252.71(8)
_cod_database_code               7041078
_chemical_oxdiff_formula         C19Ti1O1H24
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C6(H6), C2(H2), C5(H5), C4(H4), C3(H3), C10(H10), C14(H14), C15(H15),
 C11(H11), C13(H13), C9(H9), C12(H12), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              88128
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-11
_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 1.754
_oxdiff_exptl_absorpt_empirical_full_min 0.485