The Molecular and Crystal Structure of 3,5-Dimethylpyrazole with Chloranilic Acid Adduct
MARFO-OWUSU, Emmanuel; THOMPSON, Amber; X-ray Structure Analysis Online 30 (2014) 45–; doi:10.2116/xraystruct.30.45

data_1551669
_publ_section_title
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 The Molecular and Crystal Structure of 3,5-Dimethylpyrazole with
 Chloranilic Acid Adduct
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_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              45
_journal_paper_doi               10.2116/xraystruct.30.45
_journal_volume                  30
_journal_year                    2014
_chemical_formula_moiety         'C11 H10 Cl2 N2 O4'
_chemical_formula_sum            'C11 H10 Cl2 N2 O4'
_chemical_formula_weight         305.12
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 108.2971(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.67470(10)
_cell_length_b                   9.42040(10)
_cell_length_c                   13.6237(2)
_cell_measurement_reflns_used    16815
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     1300.73(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27068
_diffrn_reflns_theta_full        76.672
_diffrn_reflns_theta_max         76.672
_diffrn_reflns_theta_min         4.362
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.624
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            clear_dark_red
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2716
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.0007423
_refine_ls_shift/su_mean         0.0000671
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

 Method= Modified Sheldrick 

 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.64P] 

 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0753
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0753
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2620
_reflns_number_total             2726
_reflns_threshold_expression     I>2.0\s(I)
_iucr_refine_instructions_details_constraints
;

BLOCK SCALE X'S, U'S 

RIDE O   (  13,X'S) H   ( 131,X'S) 

RIDE C   (  21,X'S) H   ( 211,X'S) 

RIDE N   (  23,X'S) H   ( 231,X'S) 

RIDE N   (  24,X'S) H   ( 241,X'S) 

RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 

RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 273,X'S) H   ( 272,X'S) 

END                                                                             

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_iucr_refine_instructions_details_restraints
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NO 

REM   HREST   START (DO NOT REMOVE THIS LINE) 

REM   HREST   END (DO NOT REMOVE THIS LINE) 

END                                                                             

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_cod_data_source_file            30_45_1.txt
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/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 6524 2018-11-02 12:15:13Z antanas 
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_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               1551669