Synthesis and Reactivity of Low-Coordinate Titanium Synthons Supported by a Reduced Redox-Active Ligand.
Clark, Kensha Marie; Inorganic chemistry 55 (2016) 6443–6448; doi:10.1021/acs.inorgchem.6b00404

data_4344884
_publ_section_title
;
 Synthesis and Reactivity of Low-Coordinate Titanium Synthons Supported by
 a Reduced Redox-Active Ligand.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6443
_journal_page_last               6448
_journal_paper_doi               10.1021/acs.inorgchem.6b00404
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C46 H62 N2 Ti'
_chemical_formula_sum            'C46 H62 N2 Ti'
_chemical_formula_weight         690.87
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                93.342(4)
_cell_angle_beta                 96.771(4)
_cell_angle_gamma                101.354(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4606(12)
_cell_length_b                   13.0568(12)
_cell_length_c                   14.1283(15)
_cell_measurement_reflns_used    8888
_cell_measurement_temperature    200
_cell_measurement_theta_max      23.977
_cell_measurement_theta_min      2.182
_cell_volume                     2051.1(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      200
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II TXS'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47580
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.402
_diffrn_reflns_theta_min         2.166
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1382 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.7653.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'Dark Purple'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    Purple
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       Block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7513
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0526P)^2^+0.6504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6000
_reflns_number_total             7513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00404_si_002.cif
_cod_data_source_block           KCNP1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_modifier' value 'Dark' changed to 'dark'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               4344884
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.957
_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 body (RIGU) restrains
 C14, C15, C15B, C16, C16B, C17, C17B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C29(H29), C32(H32), C41(H41), C44(H44)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C25(H25), C26(H26),
 C27(H27), C37(H37), C38(H38), C39(H39)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16B(H16D,
 H16E,H16F), C17(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              60487
_shelx_hkl_checksum              44718
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'