Cooperative association of pyrazoles and phenols: A versatile binary systemElectronic supplementary information (ESI) available: Details for crystal structure determination and refinement and geometry of hydrogen bonding in structures. See http://www.rsc.org/suppdata/nj/b3/b317104c/
Boldog, Ishtvan; Rusanov, Eduard B.; Sieler, Joachim; Domasevitch, Konstantin V.; New Journal of Chemistry 28 (2004) 756–; doi:10.1039/b317104c

data_7050306
_publ_section_title
;
 Cooperative association of pyrazoles and phenols: A versatile binary
 systemElectronic supplementary information (ESI) available: Details
 for crystal structure determination and refinement and geometry of
 hydrogen bonding in structures. See
 http://www.rsc.org/suppdata/nj/b3/b317104c/
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              756
_journal_paper_doi               10.1039/b317104c
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C26 H36 N8 O4'
_chemical_formula_weight         524.63
_chemical_name_systematic
;
3,3',5,5'-Tetramethyl-4,4'-bipyrazolyl 2:1 adduct with
Floroglucine, Monohydrate
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   29.564(3)
_cell_length_b                   46.197(6)
_cell_length_c                   8.5541(10)
_cell_measurement_temperature    223(2)
_cell_volume                     11683(2)
_computing_data_reduction        'Brucker Saint'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.254
_diffrn_measured_fraction_theta_max 0.254
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15462
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.9659
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(10)
_refine_ls_extinction_coef       SHELXL
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5317
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+3.5711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                4532
_reflns_number_total             5317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b317104c.txt
_cod_data_source_block           c1027
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+3.5711P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+3.5711P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7050306