Multifaceted chelating μ-(η(3):η(3)-antifacial)-(cis-C4R2H2) coordination motif in binuclear complexes.
Liu, Cham-Chuen; Chan, Michael C. W.; Lo, Po-Kam; Lau, Kai-Chung; Yiu, Shek-Man; Chemical communications (Cambridge, England) 52 (2016) 11056–11059; doi:10.1039/c6cc05535d

data_7124922
_publ_section_title
;
 Multifaceted chelating \m-(\h(3):\h(3)-antifacial)-(cis-C4R2H2)
 coordination motif in binuclear complexes.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11056
_journal_page_last               11059
_journal_paper_doi               10.1039/c6cc05535d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C70 H78 N2 O2 Ti2'
_chemical_formula_sum            'C70 H78 N2 O2 Ti2'
_chemical_formula_weight         1075.14
_chemical_name_systematic        Ti2-H
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Dec 13 09:44:48 2013'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 92.8099(13)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.09321(15)
_cell_length_b                   22.0757(3)
_cell_length_c                   28.1078(4)
_cell_measurement_reflns_used    16884
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5439
_cell_measurement_theta_min      3.7285
_cell_volume                     6875.05(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   33.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 33

  2 omega   35.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 27

  3 omega    6.00   42.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -150.0000 36

  4 omega   42.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 35

  5 omega -115.00  -37.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000  -60.0000 78

  6 omega   78.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -180.0000 39

  7 omega   99.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   60.0000 27

  8 omega  -72.00    9.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -60.0000 81

  9 omega -113.00   -7.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000  150.0000 106

 10 omega   40.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 31

 11 omega   38.00   70.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 32

 12 omega   39.00   68.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   90.0000 29

 13 omega   38.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 25

 14 omega   38.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   60.0000 33

 15 omega   50.00  130.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  120.0000 80

 16 omega   81.00  130.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -77.0000  -60.0000 49

 17 omega   38.00   68.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -60.0000 30

 18 omega   38.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   30.0000 33

 19 omega   42.00   69.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -120.0000 27

 20 omega   41.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 30

 21 omega   38.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 25

 22 omega   76.00  121.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   60.0000 45

 23 omega  145.00  175.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   60.0000 30

 24 omega  102.00  129.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  -90.0000 27

 25 omega   43.00   95.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  -90.0000 52

 26 omega  -21.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

 27 omega  -21.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 90

 28 omega -127.00  -29.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -37.0000  120.0000 98

 29 omega -124.00  -47.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -70.0000 -136.0000 77
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0506656000
_diffrn_orient_matrix_UB_12      -0.0630246000
_diffrn_orient_matrix_UB_13      -0.0135165000
_diffrn_orient_matrix_UB_21      -0.0866262000
_diffrn_orient_matrix_UB_22      0.0037584000
_diffrn_orient_matrix_UB_23      0.0410990000
_diffrn_orient_matrix_UB_31      -0.0962456000
_diffrn_orient_matrix_UB_32      0.0297526000
_diffrn_orient_matrix_UB_33      -0.0337371000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38840
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         12262
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+1.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                10743
_reflns_number_total             12262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc05535d2.cif
_cod_data_source_block           Ti2-H_121213_ben
_cod_original_cell_volume        6875.05(17)
_cod_database_code               7124922
_cell_oxdiff_angle_alpha         90.037(2)
_cell_oxdiff_angle_beta          92.792(2)
_cell_oxdiff_angle_gamma         90.022(2)
_cell_oxdiff_length_a            11.0925(3)
_cell_oxdiff_length_b            22.0724(6)
_cell_oxdiff_length_c            28.1132(8)
_cell_oxdiff_measurement_reflns_used 16884
_cell_oxdiff_volume              6875.1(3)
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_solvent_exptl_crystal_recrystallization_method toulene/n-pentane