#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:23:43 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224246 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/12/7701255.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7701255
loop_
_publ_author_name
'Fritzsche, J.'
'Ettlinger, R.'
'Grzywa, M.'
'Jantz, S. G.'
'Kalytta-Mewes, A'
'Bunzen, H.'
'Höppe, H A'
'Volkmer, D.'
_publ_section_title
;
 CFA-15 - a perfluorinated metal-organic framework with linear 1-D
 CuII-chains containing accessible unsaturated, reactive metal
 centres.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15236
_journal_page_last               15246
_journal_paper_doi               10.1039/c9dt02133g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C6 H2 F6 N2 O2'
_chemical_formula_weight         248.10
_chemical_name_common
'3,5-bis(trifluoromethyl)pyrazole-4-carboxylic acid'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-05-02 deposited with the CCDC.    2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7891(4)
_cell_length_b                   6.9057(3)
_cell_length_c                   17.1652(9)
_cell_measurement_reflns_used    7108
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      2.373
_cell_volume                     804.76(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.530
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.530
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7108
_diffrn_reflns_point_group_measured_fraction_full 0.528
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.942
_diffrn_reflns_theta_min         2.373
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 multi-scan absorption correction using SADABS 
(G. M. Sheldrick, (1996). SADABS. Program for Empirical 
Absorption Correction. University of Göttingen, Germany.)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_description       rod
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 0 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         418
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0392P)²+11.1404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.525
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                414
_reflns_number_total             418
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02133g2.cif
_cod_data_source_block           H2-tfpc
_cod_depositor_comments
'Adding full bibliography for 7701254--7701255.cif.'
_cod_database_code               7701255
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2013-4
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
F51 F 0.0000 0.3485(3) 0.44545(16) 0.0458(17) Uani 1 2 d DS T P
F31 F 0.0000 0.3781(3) 0.0667(2) 0.0458(17) Uani 1 2 d DS T P
F52 F 0.3365(2) 0.4035(4) 0.9198(2) 0.0547(13) Uani 1 1 d . . .
F32 F 0.6505(3) 0.3980(4) 0.5771(2) 0.0547(13) Uani 1 1 d . . .
O1 O 0.0000 0.8148(14) 0.1818(6) 0.039(2) Uani 1 2 d DS T P
O2 O 0.0000 0.8122(15) 0.3107(5) 0.039(2) Uani 1 2 d DS T P
N1 N 0.0000 0.4175(4) 0.2904(4) 0.033(2) Uani 1 2 d DS T P
N2 N 0.0000 0.4226(4) 0.2131(4) 0.033(2) Uani 1 2 d DS T P
C41 C 0.0000 0.1004(18) 0.7465(6) 0.026(2) Uani 1 2 d DS T P
C4 C 0.0000 0.8890(18) 0.75139(6) 0.026(2) Uani 1 2 d DS T P
C5 C 0.0000 0.2349(3) 0.31545(8) 0.022(2) Uani 1 2 d DS T P
C3 C 0.0000 0.2394(3) 0.18879(8) 0.022(2) Uani 1 2 d DS T P
C51 C 0.0000 0.1914(2) 0.40074(9) 0.041(3) Uani 1 2 d DS T P
C31 C 0.0000 0.2076(2) 0.10268(9) 0.041(3) Uani 1 2 d DS T P
H1 H 0.0000 0.676(2) 0.1777(10) 0.050 Uiso 1 2 d DS U P
H2 H 0.0000 0.511(4) 0.3320(9) 0.050 Uiso 1 2 d DS U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C41 O1 H1 122.0(14) 2_564 .
N2 N1 C5 110.3(4) . .
N2 N1 H2 136.5(16) . .
C5 N1 H2 113.2(17) . .
N1 N2 C3 106.7(3) . .
O1 C41 O2 123.5(11) 2_565 2_565
O1 C41 C4 121.1(9) 2_565 1_545
O2 C41 C4 115.4(9) 2_565 1_545
C3 C4 C5 102.6(8) 2_565 2_565
C3 C4 C41 126.3(5) 2_565 1_565
C5 C4 C41 131.2(6) 2_565 1_565
N1 C5 C4 109.1(5) . 2_564
N1 C5 C51 120.4(3) . .
C4 C5 C51 130.5(4) 2_564 .
N2 C3 C4 111.3(5) . 2_564
N2 C3 C31 116.7(3) . .
C4 C3 C31 132.0(4) 2_564 .
F51 C51 F52 105.09(19) . 7_454
F51 C51 F52 105.09(19) . 6_554
F52 C51 F52 113.2(3) 7_454 6_554
F51 C51 C5 113.66(19) . .
F52 C51 C5 109.9(2) 7_454 .
F52 C51 C5 109.9(2) 6_554 .
F31 C31 F32 109.42(18) . 6_554
F31 C31 F32 109.42(18) . 7_454
F32 C31 F32 100.4(2) 6_554 7_454
F31 C31 C3 109.2(2) . .
F32 C31 C3 114.02(18) 6_554 .
F32 C31 C3 114.02(18) 7_454 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
F51 C51 1.3293(17) .
F31 C31 1.3294(17) .
F52 C51 1.3294(15) 6
F32 C31 1.3294(15) 6
O1 C41 1.256(11) 2_564
O1 H1 0.960(14) .
O2 C41 1.256(11) 2_564
N1 N2 1.328(9) .
N1 C5 1.332(3) .
N1 H2 0.960(13) .
N2 C3 1.332(3) .
C41 O1 1.256(11) 2_565
C41 O2 1.256(11) 2_565
C41 C4 1.462(18) 1_545
C4 C3 1.393(8) 2_565
C4 C5 1.393(8) 2_565
C4 C41 1.462(18) 1_565
C5 C4 1.393(8) 2_564
C5 C51 1.495(2) .
C3 C4 1.393(8) 2_564
C3 C31 1.495(2) .
C51 F52 1.3294(15) 7_454
C51 F52 1.3294(15) 6_554
C31 F32 1.3294(15) 6_554
C31 F32 1.3294(15) 7_454
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1 N2 0.960(14) 1.853(17) 2.761(10) 156.6(16)
N1 H2 O2 0.960(13) 2.12(3) 2.748(11) 122.1(18)
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
