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_7035108
_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         'C13 H15 Cd0.5 N2 O3, 1.8(C O)'
_chemical_formula_sum            'C14.8 H22.2 Cd0.5 N2 O4.8'
_chemical_formula_weight         361.15
_chemical_properties_physical    'Loses solvent immediately.'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.841(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.2670(4)
_cell_length_b                   21.2820(4)
_cell_length_c                   12.6080(4)
_cell_measurement_reflns_used    98871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     3553.34(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29301
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1499
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4032
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+6.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                3659
_reflns_number_total             4032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00011d2.cif
_cod_data_source_block           h11adb06
_cod_depositor_comments
'Adding full bibliography for 7035103--7035111.cif.'
_cod_original_cell_volume        3553.34(16)
_cod_original_formula_sum        'C14.80 H22.20 Cd0.50 N2 O4.80'
_cod_database_code               7035108
_olex2_refinement_description
;
1. Others
 Fixed Sof: O6(0.5) O4A(0.35) O5A(0.5) O4B(0.15) O5B(0.3) C8(0.8) C9(0.5)
 Fixed U12: Cd1(0) C10(0)
 Fixed U23: Cd1(0) C10(0)
 Fixed Uiso: H1(0.032) H2(0.034) H3(0.034) H5(0.04) H6(0.039) H11A(0.08)
 H11B(0.08) H11C(0.08) H31A(0.053) H31B(0.053) H31C(0.053) H51A(0.061)
 H51B(0.061) H51C(0.061)
 Fixed X: Cd1(0.5) H1(0.7375) H2(0.714) H3(0.6709) H5(0.8352) H6(0.8871)
 C10(1) H11A(0.4432) H11B(0.4582) H11C(0.5421) H31A(0.467) H31B(0.5226)
 H31C(0.5237) H51A(0.9057) H51B(0.9269) H51C(0.8996)
 Fixed Y: H1(0.6938) H2(0.4031) H3(0.5037) H5(0.4764) H6(0.3793) H11A(0.7488)
 H11B(0.6742) H11C(0.7181) H31A(0.584) H31B(0.5176) H31C(0.5668) H51A(0.6544)
 H51B(0.5977) H51C(0.5833)
 Fixed Z: Cd1(0.25) H1(0.3979) H2(0.0521) H3(0.0848) H5(0.4504) H6(0.4176)
 C10(0.25) H11A(-0.0879) H11B(-0.0808) H11C(0.0231) H31A(0.1212) H31B(0.1423)
 H31C(0.047) H51A(0.4984) H51B(0.4309) H51C(0.5358)
;
_olex2_submission_special_instructions 'No special instructions were received'