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_7035111
_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         '0.25(C204 H172 Cu16 N40 O32)'
_chemical_formula_sum            'C51 H43 Cu4 N10 O8'
_chemical_formula_weight         1178.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 92.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.658(4)
_cell_length_b                   13.470(3)
_cell_length_c                   18.736(4)
_cell_measurement_reflns_used    4578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.18
_cell_volume                     4705.6(18)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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     0.71080
_diffrn_reflns_av_R_equivalents  0.1242
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30696
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.18
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.722
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.461
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.520
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      2.543
_refine_ls_R_factor_all          0.3323
_refine_ls_R_factor_gt           0.2556
_refine_ls_shift/su_max          0.003
_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          0.5936
_refine_ls_wR_factor_ref         0.6441
_reflns_number_gt                2471
_reflns_number_total             4578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00011d2.cif
_cod_data_source_block           i2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035103--7035111.cif.
;
_cod_original_cell_volume        4705.6(16)
_cod_database_code               7035111
_olex2_refinement_description
;
1. Others
 Fixed Sof: O1(0.5) O1A(0.5) O1B(0.5) O1C(0.5) N1(0.5) N1A(0.5) N1B(0.5)
 N1C(0.5) O2(0.5) O2A(0.5) O2B(0.5) O2C(0.5) N2B(0.5) N2C(0.5) C3'(0.5)
 C3A'(0.5) C3C'(0.5) C4C'(0.5) C7(0.5) C7A(0.5) C7B(0.5) C7C(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) H31C(0.5) C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5)
 C31B(0.5) H31G(0.5) H31H(0.5) H31I(0.5) C31C(0.5) H31J(0.5) H31K(0.5)
 H31L(0.5) C51C(0.5) H51G(0.5) H51H(0.5) H51I(0.5)
 Fixed Uiso: H2(0.069) H2B(0.073) H3(0.057) H3B(0.058) H5(0.039) H5B(0.051)
 H6(0.055) H6B(0.068) H31A(0.069) H31B(0.069) H31C(0.069) H31D(0.111)
 H31E(0.111) H31F(0.111) H31G(0.072) H31H(0.072) H31I(0.072) H31J(0.124)
 H31K(0.124) H31L(0.124) H51A(0.163) H51B(0.163) H51C(0.163) H51D(0.16)
 H51E(0.16) H51F(0.16) H51G(0.097) H51H(0.097) H51I(0.097)
 Fixed X: H2(0.4297) H2B(0.7971) H3(0.4831) H3B(0.8309) H5(0.665) H5B(0.9135)
 H6(0.6065) H6B(0.8909) H31A(0.5644) H31B(0.6179) H31C(0.6447) H31D(0.5785)
 H31E(0.6638) H31F(0.623) H31G(1.0368) H31H(1.0514) H31I(1.0243) H31J(1.064)
 H31K(1.045) H31L(1.0178) H51A(0.6555) H51B(0.7232) H51C(0.6464) H51D(0.7357)
 H51E(0.7306) H51F(0.7407) H51G(0.768) H51H(0.7511) H51I(0.7485)
 Fixed Y: H2(0.8336) H2B(1.0113) H3(0.9882) H3B(0.874) H5(0.8829) H5B(0.7592)
 H6(0.7343) H6B(0.9194) H31A(1.0599) H31B(1.1412) H31C(1.0295) H31D(1.0632)
 H31E(1.0616) H31F(0.9661) H31G(0.7337) H31H(0.6172) H31I(0.6807) H31J(0.7003)
 H31K(0.7672) H31L(0.7996) H51A(1.0097) H51B(1.0821) H51C(1.1259) H51D(0.719)
 H51E(0.6071) H51F(0.6965) H51G(0.5795) H51H(0.5732) H51I(0.6781)
 Fixed Z: H2(0.6505) H2B(0.6377) H3(0.6706) H3B(0.5746) H5(0.5857) H5B(0.7619)
 H6(0.5561) H6B(0.813) H31A(0.7664) H31B(0.8008) H31C(0.7901) H31D(0.8127)
 H31E(0.8249) H31F(0.7928) H31G(0.6024) H31H(0.6114) H31I(0.6774) H31J(0.5877)
 H31K(0.655) H31L(0.5764) H51A(0.4996) H51B(0.5085) H51C(0.4843) H51D(0.6105)
 H51E(0.582) H51F(0.527) H51G(0.6779) H51H(0.5937) H51I(0.6337)
;
_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'