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_7041081
_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         'C14 H19 Cl Hf O'
_chemical_formula_sum            'C14 H19 Cl Hf O'
_chemical_formula_weight         417.23
_chemical_name_systematic
bis(cyclopentadienyl)hafnium(cloro)(tert-butoxide)
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-16
_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                   15.2640(3)
_cell_length_b                   12.0177(3)
_cell_length_c                   15.8499(5)
_cell_measurement_reflns_used    11579
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5270
_cell_measurement_theta_min      3.6250
_cell_volume                     2907.48(13)
_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      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 0.998
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w     -1.00  87.00   1.00   10.00    --   17.57  38.00  90.00   88
  2  \w      1.00  85.00   1.00   10.00    --   17.57  57.00-150.00   84
  3  \w      1.00  85.00   1.00   10.00    --   17.57  57.00 -30.00   84
  4  \w      1.00  85.00   1.00   10.00    --   17.57  57.00 150.00   84
  5  \w    -50.00  44.00   1.00   10.00    --   17.57 -77.00  60.00   94
  6  \w    -50.00  34.00   1.00   10.00    --   17.57 -57.00 -60.00   84
  7  \w    -50.00  44.00   1.00   10.00    --   17.57 -77.00-180.00   94
  8  \w    -52.00 -23.00   1.00   10.00    --   17.57 -38.00  60.00   29
;
_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      0.0331609000
_diffrn_orient_matrix_UB_12      -0.0079787000
_diffrn_orient_matrix_UB_13      0.0307485000
_diffrn_orient_matrix_UB_21      -0.0297566000
_diffrn_orient_matrix_UB_22      -0.0309111000
_diffrn_orient_matrix_UB_23      0.0251151000
_diffrn_orient_matrix_UB_31      0.0132220000
_diffrn_orient_matrix_UB_32      -0.0496758000
_diffrn_orient_matrix_UB_33      -0.0205909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.829
_diffrn_reflns_theta_min         3.162
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.342
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.498
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.312
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0170P)^2^+9.0550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3356
_reflns_number_total             3899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03199d2.cif
_cod_data_source_block           nb04
_cod_depositor_comments
'Adding full bibliography for 7041078--7041081.cif.'
_cod_original_cell_volume        2907.49(13)
_cod_database_code               7041081
_chemical_oxdiff_formula         C14H19Cl1Hf1O1
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              19128
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-16
_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 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.814