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_7124924
_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         'C72 H82 Hf2 N2 O2, 0.5(C3 H7)'
_chemical_formula_sum            'C73.5 H85.5 Hf2 N2 O2'
_chemical_formula_weight         1385.92
_chemical_name_systematic        Hf2-Me
_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
;
'Wed Apr 24 10:13:49 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                 103.614(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.6909(3)
_cell_length_b                   16.2174(3)
_cell_length_c                   27.5623(6)
_cell_measurement_reflns_used    16358
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6114
_cell_measurement_theta_min      3.1434
_cell_volume                     6382.2(2)
_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      133(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   -9.00   21.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  120.0000 30

  2 omega   32.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 31

  3 omega  -25.00   34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 59

  4 omega -112.00  -39.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000 -180.0000 73

  5 omega -124.00  -38.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000    0.0000 86

  6 omega  -63.00    0.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000 -180.0000 63

  7 omega  -64.00   -7.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000  -30.0000 57

  8 omega   37.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 29

  9 omega   38.00   64.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 26

 10 omega   45.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 26

 11 omega   44.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  -60.0000 46

 12 omega   42.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  150.0000 26

 13 omega   40.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 32

 14 omega   47.00   87.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  120.0000 40

 15 omega   40.00   77.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   30.0000 37

 16 omega   48.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -180.0000 35

 17 omega   56.00   88.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   60.0000 32

 18 omega   40.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 26

 19 omega   40.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 30

 20 omega   55.00   80.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   60.0000 25

 21 omega   95.00  152.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  150.0000 57

 22 omega   52.00   77.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000 -120.0000 25

 23 omega   43.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   90.0000 47

 24 omega   38.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  -30.0000 52
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0878041000
_diffrn_orient_matrix_UB_12      0.0454302000
_diffrn_orient_matrix_UB_13      0.0295781000
_diffrn_orient_matrix_UB_21      -0.0610807000
_diffrn_orient_matrix_UB_22      0.0746077000
_diffrn_orient_matrix_UB_23      0.0064604000
_diffrn_orient_matrix_UB_31      -0.0149951000
_diffrn_orient_matrix_UB_32      -0.0372466000
_diffrn_orient_matrix_UB_33      0.0488728000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27507
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    6.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54140
_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            indigo
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2802
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11381
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0319P)^2^+10.6768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                11139
_reflns_number_total             11381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc05535d2.cif
_cod_data_source_block           Hf2-Me_042313a_ben
_cod_original_formula_sum        'C73.50 H85.50 Hf2 N2 O2'
_cod_database_code               7124924
_cell_oxdiff_angle_alpha         90.071(2)
_cell_oxdiff_angle_beta          103.691(2)
_cell_oxdiff_angle_gamma         89.931(2)
_cell_oxdiff_length_a            14.6808(4)
_cell_oxdiff_length_b            16.2232(5)
_cell_oxdiff_length_c            27.5805(7)
_cell_oxdiff_measurement_reflns_used 16358
_cell_oxdiff_volume              6382.2(3)
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_solvent_exptl_crystal_recrystallization_method benzene/n-pentane