The synthesis and characterisation of coordination and hydrogen-bonded networks based on 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid.
Bryant, Macguire R.; Burrows, Andrew D.; Fitchett, Christopher M.; Hawes, Chris S.; Hunter, Sally O.; Keenan, Luke L.; Kelly, David J.; Kruger, Paul E.; Mahon, Mary F.; Richardson, Christopher; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9269–9280; doi:10.1039/c5dt00011d

data_7035110
_publ_section_title
;
 The synthesis and characterisation of coordination and hydrogen-bonded
 networks based on 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9269
_journal_page_last               9280
_journal_paper_doi               10.1039/c5dt00011d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '0.13(C192 H176 Cu8 N32 O32), 4(C H4 O), O'
_chemical_formula_sum            'C28 H38 Cu N4 O9'
_chemical_formula_weight         638.16
_chemical_properties_physical
'Crystals lose solvent and change to another phase.'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_Int_Tables_number      88
_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     iterative
_audit_creation_date             2014-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-03-12 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5927(4)
_cell_length_b                   23.5927(4)
_cell_length_c                   11.7356(3)
_cell_measurement_reflns_used    6699
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7460
_cell_measurement_theta_min      4.1870
_cell_volume                     6532.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -49.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563   37.0000 -120.0000 85

  2 omega   41.00   74.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6563 -125.0000  -90.0000 33

  3 omega -119.00  -92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000    0.0000 27

  4 omega  132.00  168.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000   30.0000 36

  5 omega   31.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -90.0000 32

  6 omega   33.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 45

  7 omega   80.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000  150.0000 97

  8 omega -118.00   -6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -77.0000  120.0000 112

  9 omega -116.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -37.0000 -120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0569727000
_diffrn_orient_matrix_UB_12      0.0306468000
_diffrn_orient_matrix_UB_13      -0.0178507000
_diffrn_orient_matrix_UB_21      0.0300988000
_diffrn_orient_matrix_UB_22      -0.0455879000
_diffrn_orient_matrix_UB_23      0.0719933000
_diffrn_orient_matrix_UB_31      0.0108123000
_diffrn_orient_matrix_UB_32      -0.0352272000
_diffrn_orient_matrix_UB_33      -0.1083051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.920
_diffrn_reflns_theta_min         4.208
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1153P)^2^+18.7110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2962
_reflns_number_total             3092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00011d2.cif
_cod_data_source_block           55crw
_cod_depositor_comments
'Adding full bibliography for 7035103--7035111.cif.'
_cod_original_cell_volume        6532.2(3)
_cod_database_code               7035110
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: O16(0.5)
 Fixed Uiso: H1(0.027) H6(0.03) H5(0.03) H3(0.03) H14(0.052) H31A(0.043)
 H31B(0.043) H31C(0.043) H2(0.031) H51A(0.048) H51B(0.048) H51C(0.048)
 H10(0.142) H11A(0.127) H11B(0.127) H11C(0.127) H12(0.294) H15A(0.109)
 H15B(0.109) H15C(0.109) H13A(0.155) H13B(0.155) H13C(0.155)
 Fixed X: Cu1(0.5) H1(0.1925) H6(0.3969) H5(0.3405) H3(0.3138) H14(0.3679)
 H31A(0.1591) H31B(0.2029) H31C(0.2065) H2(0.3704) H51A(0.3659) H51B(0.3877)
 H51C(0.3525) H10(0.5244) H11A(0.432) H11B(0.4546) H11C(0.4634) H12(0.4294)
 H15A(0.4536) H15B(0.44) H15C(0.3939) H13A(0.4432) H13B(0.4681) H13C(0.4283)
 Fixed Y: Cu1(0.5) H1(0.6441) H6(0.6164) H5(0.661) H3(0.5116) H14(0.6346)
 H31A(0.5685) H31B(0.5444) H31C(0.5264) H2(0.4672) H51A(0.7234) H51B(0.68)
 H51C(0.7331) H10(0.5768) H11A(0.5821) H11B(0.5652) H11C(0.5242) H12(0.6232)
 H15A(0.6926) H15B(0.6353) H15C(0.6831) H13A(0.6942) H13B(0.6448) H13C(0.6901)
 Fixed Z: Cu1(0.5) H1(-0.174) H6(0.3047) H5(0.1712) H3(0.0154) H14(0.5945)
 H31A(-0.0434) H31B(0.0447) H31C(-0.0837) H2(0.1489) H51A(-0.1259) H51B(-
 0.0347) H51C(0.0035) H10(-0.1635) H11A(-0.1196) H11B(0.0013) H11C(-0.1024)
 H12(0.5239) H15A(0.6417) H15B(0.7037) H15C(0.6973) H13A(0.5028) H13B(0.5768)
 H13C(0.6328)
;
_olex2_submission_special_instructions 'No special instructions were received'