Construction of extended networks with a trimeric pyrazole synthon
Boldog, Ishtvan; Rusanov, Eduard B.; Sieler, Joachim; Blaurock, Steffen; Domasevitch, Konstantin V.; Chemical Communications (Cambridge, United Kingdom)  (2003) 740–741; doi:10.1039/b212540d

data_7104020
_publ_section_title
;
 Construction of extended networks with a trimeric pyrazole synthon
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   6
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
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_journal_page_first              740
_journal_page_last               741
_journal_paper_doi               10.1039/b212540d
_journal_year                    2003
_chemical_formula_sum            'C10 H14 N4'
_chemical_formula_weight         190.25
_chemical_name_common
'3,3',5,5'-Tetramethyl-4,4'-Bipyrazole, Tetragonal form ('
_chemical_name_systematic
;
3,3',5,5'-Tetramethyl-4,4'-Bipyrazole, Tetragonal form (#3)
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_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            24
_cell_length_a                   27.619(3)
_cell_length_b                   27.619(3)
_cell_length_c                   8.6029(11)
_cell_measurement_temperature    223(2)
_cell_volume                     6562.5(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'SMART CCD Siemens'
_diffrn_measurement_method       'omega scnans'
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19799
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'slightly yellowish'
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3.04(230)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.164
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2960
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.300
_refine_ls_restrained_S_obs      1.189
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+1.1537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1256
_refine_ls_wR_factor_obs         0.1034
_reflns_number_observed          2645
_reflns_number_total             3706
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b212540d.txt
_cod_data_source_block           c1214
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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^)+(0.0564P)^2^+1.1537P] 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^)+(0.0564P)^2^+1.1537P] 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      I4(1)cd
_cod_database_code               7104020