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_7035109
_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         'C24 H26 Cu2 N4 O10 S'
_chemical_formula_sum            'C24 H26 Cu2 N4 O10 S'
_chemical_formula_weight         689.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 103.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.685(7)
_cell_length_b                   29.520(6)
_cell_length_c                   9.7350(19)
_cell_measurement_temperature    100(2)
_cell_volume                     9125(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71083
_diffrn_reflns_av_R_equivalents  0.1489
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            42241
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.28
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.430
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5882
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2701
_refine_ls_wR_factor_ref         0.2914
_reflns_number_gt                3883
_reflns_number_total             5882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00011d2.cif
_cod_data_source_block           c2m-sr
_cod_depositor_comments
'Adding full bibliography for 7035103--7035111.cif.'
_cod_database_code               7035109
_olex2_refinement_description
;
1. Others
 Fixed U12: Cu2(0) Cu3(0) O8(0) O9(0)
 Fixed U23: Cu2(0) Cu3(0) O8(0) O9(0)
 Fixed Uiso: H7A(0.163) H7B(0.163) H8A(0.16) H8B(0.16) H9A(0.183) H9B(0.183)
 H1(0.069) H1A(0.072) H2(0.101) H2A(0.082) H3(0.086) H3A(0.092) H5(0.094)
 H5A(0.071) H6(0.102) H6A(0.065) H31A(0.116) H31B(0.116) H31C(0.116)
 H31D(0.134) H31E(0.134) H31F(0.134) H51A(0.085) H51B(0.085) H51C(0.085)
 H51D(0.134) H51E(0.134) H51F(0.134)
 Fixed X: H7A(0.166) H7B(0.2074) H1(0.2762) H1A(0.1531) H2(0.4449) H2A(0.0098)
 H3(0.3967) H3A(0.0462) H5(0.346) H5A(0.1504) H6(0.394) H6A(0.1146)
 H31A(0.2825) H31B(0.3289) H31C(0.2891) H31D(0.2104) H31E(0.1711) H31F(0.2055)
 H51A(0.3205) H51B(0.3672) H51C(0.3372) H51D(0.0895) H51E(0.0784) H51F(0.0574)
 Fixed Y: Cu2(0) Cu3(0) H7A(0.1737) H7B(0.1581) O8(0) H8A(0) H8B(0) O9(0)
 H9A(0) H9B(0) H1(0.257) H1A(0.255) H2(0.0809) H2A(0.1064) H3(0.1338)
 H3A(0.1519) H5(0.1556) H5A(0.1359) H6(0.1114) H6A(0.0885) H31A(0.1204)
 H31B(0.1069) H31C(0.0966) H31D(0.1174) H31E(0.0946) H31F(0.1219) H51A(0.2521)
 H51B(0.2456) H51C(0.2841) H51D(0.2812) H51E(0.2542) H51F(0.2395)
 Fixed Z: H7A(-0.2995) H7B(-0.3396) H1(-0.2718) H1A(-0.0796) H2(-0.1698)
 H2A(0.1508) H3(-0.1091) H3A(0.0171) H5(-0.5188) H5A(0.335) H6(-0.5864)
 H6A(0.4491) H31A(-0.0587) H31B(-0.0717) H31C(-0.1996) H31D(0.0329)
 H31E(0.0776) H31F(0.192) H51A(-0.4975) H51B(-0.4017) H51C(-0.3632) H51D(-
 0.0127) H51E(0.1162) H51F(-0.0432)
;
_olex2_computing_structure_refinement_long 'SHELXL-97 (Sheldrick, 1997)'
_olex2_computing_structure_solution_long 'SHELXS-97 (Sheldrick, 1997)'
_olex2_submission_special_instructions 'No special instructions were received'