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_4109937
_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            'C46 H54 Cl8 N4 O12 Zn'
_chemical_formula_weight         1203.92
_chemical_name_systematic
; 
Dichloro[bis(3,5-bis(3',4',5'-trimethoxyphenyl)pyrazole-1-yl)methane]zinc(II)
;
_space_group_IT_number           2
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_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
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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                92.625(2)
_cell_angle_beta                 99.990(2)
_cell_angle_gamma                97.269(2)
_cell_formula_units_Z            2
_cell_length_a                   10.98830(3)
_cell_length_b                   13.2389(3)
_cell_length_c                   18.4296(5)
_cell_measurement_reflns_used    10641
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.5662
_cell_measurement_theta_min      2.8149
_cell_volume                     2612.83(10)
_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
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
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_computing_data_reduction
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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 0.825
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_details
;
  1 omega  -13.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   89.0000  -75.0000    0.0000    0.0000 51

  2 omega  -13.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   89.0000 -169.0000    0.0000    0.0000 51

  3 omega  -61.00   -9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   89.0000  104.0000    0.0000    0.0000 52

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

  5 omega  -38.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -89.0000  -10.0000    0.0000    0.0000 52

  6 omega    9.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865 -144.0000  103.0000    0.0000    0.0000 44

  7 omega   10.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -89.0000 -104.0000    0.0000    0.0000 51

  8 omega  -53.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   75.0000    0.0000    0.0000    0.0000 54
;
_diffrn_orient_matrix_UB_11      0.0424629062
_diffrn_orient_matrix_UB_12      -0.0334062466
_diffrn_orient_matrix_UB_13      0.0144278471
_diffrn_orient_matrix_UB_21      -0.0505619084
_diffrn_orient_matrix_UB_22      -0.0358581137
_diffrn_orient_matrix_UB_23      0.0056761056
_diffrn_orient_matrix_UB_31      -0.0040173260
_diffrn_orient_matrix_UB_32      -0.0230489282
_diffrn_orient_matrix_UB_33      -0.0359950588
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17658
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
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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            colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         8843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                6909
_reflns_number_total             8843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073639csi20070521_114246.cif
_cod_data_source_block           24
_cod_original_cell_volume        2612.83(9)
_cod_database_code               4109937