Tetrahedral Zinc Complexes with Liquid Crystalline and Luminescent Properties: Interplay Between Nonconventional Molecular Shapes and Supramolecular Mesomorphic Order
Emma Cavero; Santiago Uriel; Pilar Romero; José Luis Serrano; Raquel Giménez; Journal of the American Chemical Society 129 (2007) 11608–11618; doi:10.1021/ja073639c

data_4109938
_publ_contact_author_address
;
Departamento de Quimica Org\'anica, Centro Polit\'ecnico Superior - 
Instituto de Ciencia de Materiales de Arag\'on. Universidad de Zaragoza - CSIC,
C/ Mar\'ia de Luna 3, 50015 Zaragoza, Spain.
;
_publ_contact_author_email       suriel@unizar.es
_publ_contact_author_phone       +34976762397
_publ_section_title
;
 Tetrahedral Zinc Complexes with Liquid Crystalline and Luminescent
 Properties: Interplay Between Nonconventional Molecular Shapes and
 Supramolecular Mesomorphic Order
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11608
_journal_page_last               11618
_journal_paper_doi               10.1021/ja073639c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C43 H50 Cl4 N4 O12 Zn'
_chemical_formula_weight         1022.04
_chemical_name_systematic
; 
Dichlorobis(3,5-bis(3,4,5-trimethoxyphenyl)-1H-pyrazole)zinc(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_cell_angle_alpha                80.091(4)
_cell_angle_beta                 69.480(4)
_cell_angle_gamma                74.809(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8967(4)
_cell_length_b                   14.5460(7)
_cell_length_c                   16.0768(9)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.7526
_cell_measurement_theta_min      2.7888
_cell_volume                     2294.1(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'BRUKER SHELXTL'
_computing_structure_solution    'BRUKER SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_details
;
  1 omega  -63.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   94.0000 -138.0000    0.0000    0.0000 49

  2 omega  -62.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   91.0000  -23.0000    0.0000    0.0000 50

  3 omega  -62.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   91.0000  137.0000    0.0000    0.0000 50

  4 omega  -18.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   94.0000 -138.0000    0.0000    0.0000 49

  5 omega  -48.00    4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   45.0000  240.0000    0.0000    0.0000 52

  6 omega  -53.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   75.0000  120.0000    0.0000    0.0000 54

  7 omega   -3.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -45.0000    0.0000    0.0000    0.0000 52

  8 phi    -62.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -21.1177    0.0000     -        0.0000    0.0000 64

  9 phi    -32.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -21.1177    0.0000     -        0.0000    0.0000 64

;
_diffrn_orient_matrix_UB_11      0.0399384063
_diffrn_orient_matrix_UB_12      -0.0457581864
_diffrn_orient_matrix_UB_13      0.0069349954
_diffrn_orient_matrix_UB_21      0.0056829067
_diffrn_orient_matrix_UB_22      -0.0108674605
_diffrn_orient_matrix_UB_23      -0.0426593840
_diffrn_orient_matrix_UB_31      0.0585673702
_diffrn_orient_matrix_UB_32      0.0187871576
_diffrn_orient_matrix_UB_33      -0.0190123929
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.1303
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18149
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
ABSPack
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
?
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       Block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                4207
_reflns_number_total             7673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073639csi20070606_115200.cif
_cod_data_source_block           18
_cod_original_cell_volume        2294.06(19)
_cod_database_code               4109938