Supramolecular Structures and Columnar Mesophase Induction in Nondiscoid Pyrazoles by Complexation to Rhodium(I)
Giménez, Raquel; Elduque, Anabel; López, José Antonio; Barberá, Joaquín; Cavero, Emma; Lantero, Ignacio; Oro, Luis A.; Serrano, José Luis; Inorganic Chemistry 45 (2006) 10363–10370; doi:10.1021/ic0614216

data_4333105
_publ_section_title
;
 Supramolecular Structures and Columnar Mesophase Induction in Nondiscoid
 Pyrazoles by Complexation to Rhodium(I)
;
_journal_issue                   25
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10363
_journal_page_last               10370
_journal_paper_doi               10.1021/ic0614216
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C21 H24 N2 O6'
_chemical_formula_sum            'C21 H24 N2 O6'
_chemical_formula_weight         400.42
_chemical_name_systematic        3,5-bis(3,4,5-trimethoxyphenyl)pyrazole
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   21.2193(16)
_cell_length_b                   21.2193(16)
_cell_length_c                   18.4841(14)
_cell_measurement_reflns_used    3027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.41
_cell_volume                     8322.6(11)
_computing_cell_refinement       'SAINT+ v. 6.22 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.22 (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, 
J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_computing_structure_solution
;
SIR97 - A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, 
C. Giacovazzo, A. Guagliardi, A. G. G.  Moliterni, G. Polidori, 
R. Spagna, J. Appl. Cryst. (1999) 32, 115-119.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21937
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS: Area-Detector Absorption Correction.  v. 2.03 Bruker-AXS 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+5.1628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                2899
_reflns_number_total             3768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0614216sup1.cif
_cod_data_source_block           compound_L6
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4333105