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_7113759
_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)
;
_journal_page_first              740
_journal_page_last               741
_journal_paper_doi               10.1039/b212540d
_journal_year                    2003
_chemical_formula_sum            'C11 H15 Cl3 N4'
_chemical_formula_weight         309.62
_chemical_name_common
'3,3',5,5'-tetramethyl-4,4'-bipyrazole Chloroform solvate'
_chemical_name_systematic
;
3,3',5,5'-tetramethyl-4,4'-bipyrazole Chloroform solvate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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            48
_cell_length_a                   29.196(2)
_cell_length_b                   29.196(2)
_cell_length_c                   22.406(2)
_cell_measurement_temperature    173(2)
_cell_volume                     19099(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'IPDS Stoe'
_diffrn_measurement_method       'phi rotation'
_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  0.1213
_diffrn_reflns_av_sigmaI/netI    0.2676
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16913
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             7680
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0110(20)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.844
_refine_ls_goodness_of_fit_obs   1.553
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.623
_refine_ls_R_factor_all          0.3327
_refine_ls_R_factor_obs          0.1270
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4376
_refine_ls_wR_factor_obs         0.2836
_reflns_number_observed          1408
_reflns_number_total             7333
_reflns_observed_criterion       >2sigma(I)
_cod_duplicate_entry             7104019
_cod_data_source_file            b212540d.txt
_cod_data_source_block           dpzn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+0.0000P] 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^)+(0.1430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        19099.1(25)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7113759