Bonding in Complexes of Bis(pentalene)dititanium, Ti2(C8H6)2.
Kilpatrick, Alexander F. R.; Green, Jennifer C.; Cloke, F Geoffrey N; Organometallics 34 (2015) 4830–4843; doi:10.1021/acs.organomet.5b00363

data_4086035
_publ_section_title
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 Bonding in Complexes of Bis(pentalene)dititanium, Ti2(C8H6)2.
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4830
_journal_page_last               4843
_journal_paper_doi               10.1021/acs.organomet.5b00363
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C52 H92 Si4 Ti2, B C24 F20, 0.5(C6 H14)'
_chemical_formula_sum            'C79 H99 B F20 Si4 Ti2'
_chemical_formula_weight         1647.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                89.30(3)
_cell_angle_beta                 88.71(3)
_cell_angle_gamma                67.67(3)
_cell_formula_units_Z            2
_cell_length_a                   14.217(3)
_cell_length_b                   15.491(3)
_cell_length_c                   19.366(4)
_cell_measurement_reflns_used    57859
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     3944.2(16)
_computing_cell_refinement
;

CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)

;
_computing_data_collection
;

CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)

;
_computing_data_reduction
;

CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)

;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009) and WinGX  (Farrugia, 2012) publication routines
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61748
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-Scan (Blessing, 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1716
_exptl_crystal_preparation       'synthesis as described'
_exptl_crystal_recrystallization_method 'from Et2O/hexane solution at -35 C'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         16087
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0944P)^2^+1.4488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11947
_reflns_number_total             16087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00363_si_002.cif
_cod_data_source_block           2014ncs0267
_cod_depositor_comments
;Adding full bibliography for 4086035.cif.

 Adding full bibliography for 4086035.cif.
;
_cod_original_cell_volume        3944.1(16)
_cod_database_code               4086035
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C100, C101, C102
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C100 \\sim C101 \\sim C102: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.1
4.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C15(H15), C18(H18), C21(H21), C24(H24), C35(H35), C38(H38),
 C41(H41), C44(H44), C47(H47), C50(H50)
4.b Secondary CH2 refined with riding coordinates:
 C101(H10G,H10H), C102(H10I,H10J)
4.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C100(H10D,H10E,H10F)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C28(H28), C29(H29), C32(H32), C33(H33)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'