Nonagostic M···H‒C Interactions. Synthesis, Characterization, and DFT Study of the Titanium Amide Ti2Cl6[N(t-Bu)2]2
Spicer, Charles W.; Lovitt, Charity Flener; Girolami, Gregory S.; Organometallics 31 (2012) 4894–; doi:10.1021/om300483v

data_4078877
_publ_section_title
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 Nonagostic M&#x00B7;&#x00B7;&#x00B7;H--C Interactions. Synthesis,
 Characterization, and DFT Study of the Titanium Amide Ti2Cl6[N(t-Bu)2]2
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4894
_journal_paper_doi               10.1021/om300483v
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C16 H36 Cl6 N2 Ti2'
_chemical_formula_weight         564.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.484(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.512(2)
_cell_length_b                   20.436(7)
_cell_length_c                   8.291(3)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.29
_cell_measurement_theta_min      1.99
_cell_volume                     1272.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11813
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.80753
_exptl_absorpt_correction_T_min  0.68884
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         3080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.7820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                2561
_reflns_number_total             3080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300483v_si_003.cif
_cod_data_source_block           f04aface
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1272.8(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078877