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_7124923
_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 Zr2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C72 H83 N2 O2.5 Zr2'
_chemical_formula_weight         1198.84
_chemical_name_systematic        Zr2-H
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-12
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                79.469(2)
_cell_angle_beta                 79.993(2)
_cell_angle_gamma                81.353(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3506(3)
_cell_length_b                   15.5365(5)
_cell_length_c                   19.1544(6)
_cell_measurement_reflns_used    14861
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5719
_cell_measurement_theta_min      3.4480
_cell_volume                     3245.81(17)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   34.00   60.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 26

  2 omega   -5.00   25.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000   90.0000 30

  3 omega    1.00   35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 34

  4 omega  -69.00  -30.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 39

  5 omega  -13.00   20.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 33

  6 omega   43.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000   90.0000 29

  7 omega  -65.00   10.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000   57.0000  -90.0000 75

  8 omega -123.00  -30.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -37.0000  120.0000 93

  9 omega   73.00  126.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  120.0000 53

 10 omega   -8.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -37.0000    0.0000 79

 11 omega   73.00  126.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   60.0000 53

 12 omega   49.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -77.0000   60.0000 36

 13 omega -113.00  -45.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000   30.0000 68

 14 omega  -71.00  -27.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -60.0000 44

 15 omega   44.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000   60.0000 38

 16 omega   42.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -30.0000 29

 17 omega   38.00  153.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000   30.0000 115

 18 omega   43.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 28

 19 omega   42.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000 -180.0000 46

 20 omega   38.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   30.0000 32

 21 omega   52.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -12.0000 53

 22 omega   38.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 25

 23 omega   42.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -60.0000 29

 24 omega   42.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 27

 25 omega   92.00  131.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000 -180.0000 39

 26 omega   76.00  148.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000 -120.0000 72

 27 omega   81.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   44.0000 27

 28 omega   39.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 31

 29 omega   98.00  141.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   90.0000 43

 30 omega   97.00  141.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 44

 31 omega   45.00   73.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 28

 32 omega   38.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 32

 33 omega   40.00   65.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 25

 34 omega   38.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 25

 35 omega  105.00  131.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000   60.0000 26

 36 omega   41.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  154.0000 67

 37 omega   51.00  127.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   23.0000 76

 38 omega   88.00  171.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000 -120.0000 83

 39 omega   71.00  134.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -126.0000 63
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0853449000
_diffrn_orient_matrix_UB_12      0.0672176000
_diffrn_orient_matrix_UB_13      0.0408822000
_diffrn_orient_matrix_UB_21      -0.0091858000
_diffrn_orient_matrix_UB_22      -0.0696897000
_diffrn_orient_matrix_UB_23      0.0685357000
_diffrn_orient_matrix_UB_31      0.1091604000
_diffrn_orient_matrix_UB_32      0.0308548000
_diffrn_orient_matrix_UB_33      0.0218855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24742
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38629
_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            orange
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1258
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.218
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         11537
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+2.4761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                10741
_reflns_number_total             11537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc05535d2.cif
_cod_data_source_block           Zr2-H_090513a_ben
_cod_original_formula_sum        'C72 H83 N2 O2.50 Zr2'
_cod_database_code               7124923
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_solvent_exptl_crystal_recrystallization_method 'diethyl ether/n-pentane'