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_7035107
_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_absolute_configuration unk
_chemical_formula_moiety         'C24 H22 Co N4 O4'
_chemical_formula_sum            'C24 H22 Co N4 O4'
_chemical_formula_weight         489.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_Int_Tables_number      122
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   14.85742(19)
_cell_length_b                   14.85742(19)
_cell_length_c                   39.7127(9)
_cell_measurement_reflns_used    5188
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      73.5597
_cell_measurement_theta_min      3.1732
_cell_volume                     8766.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -74.00   21.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   77.0000 -150.0000 95

  2 omega   54.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313   77.0000    0.0000 26

  3 omega  103.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000 -120.0000 75

  4 omega  124.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000  120.0000 54

  5 omega   83.00  139.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000   30.0000 56

  6 omega  126.00  163.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   77.0000    0.0000 37

  7 omega -114.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -57.0000  150.0000 104

  8 omega -114.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -57.0000  -90.0000 104

  9 omega   33.00  105.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000  -30.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0169132000
_diffrn_orient_matrix_UB_12      -0.0089847000
_diffrn_orient_matrix_UB_13      0.0381158000
_diffrn_orient_matrix_UB_21      -0.0259842000
_diffrn_orient_matrix_UB_22      -0.0995588000
_diffrn_orient_matrix_UB_23      -0.0049057000
_diffrn_orient_matrix_UB_31      0.0989675000
_diffrn_orient_matrix_UB_32      -0.0276145000
_diffrn_orient_matrix_UB_33      0.0051909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            13939
_diffrn_reflns_theta_full        65.50
_diffrn_reflns_theta_max         65.50
_diffrn_reflns_theta_min         3.18
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0855P)^2^+3.7978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                3286
_reflns_number_total             3736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00011d2.cif
_cod_data_source_block           csh194
_cod_depositor_comments
'Adding full bibliography for 7035103--7035111.cif.'
_cod_original_cell_volume        8766.3(2)
_cod_database_code               7035107
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed U13: Co1(0) Co1A(0)
 Fixed U23: Co1(0) Co1A(0)
 Fixed Uiso: H31A(0.037) H31B(0.037) H31C(0.037) H51D(0.032) H51E(0.032)
 H51F(0.032) H31D(0.034) H31E(0.034) H31F(0.034) H51A(0.033) H51B(0.033)
 H51C(0.033) H2A(0.022) H3A(0.023) H6(0.027) H3(0.023) H5A(0.024) H5(0.024)
 H6A(0.023) H2(0.024) H1A(0.024) H1(0.024)
 Fixed X: Co1(0.5) Co1A(0.5) H31A(0.3255) H31B(0.3817) H31C(0.3795)
 H51D(0.2494) H51E(0.2647) H51F(0.3295) H31D(0.059) H31E(0.1196) H31F(0.0247)
 H51A(0.7047) H51B(0.6343) H51C(0.6784) H2A(0.3239) H3A(0.352) H6(0.4039)
 H3(0.1154) H5A(0.6197) H5(0.3477) H6A(0.5916) H2(0.1765)
 Fixed Y: Co1(1) Co1A(1) H31A(0.6027) H31B(0.5558) H31C(0.5115) H51D(1.2182)
 H51E(1.1859) H51F(1.1501) H31D(0.8499) H31E(0.8372) H31F(0.8876) H51A(0.7492)
 H51B(0.8307) H51C(0.7954) H2A(0.7832) H3A(0.7249) H6(1.0315) H3(0.926)
 H5A(0.7385) H5(1.0472) H6A(0.8041) H2(0.8991)
 Fixed Z: H31A(0.4168) H31B(0.4464) H31C(0.4097) H51D(0.5987) H51E(0.5607)
 H51F(0.59) H31D(0.6039) H31E(0.5709) H31F(0.5684) H51A(0.4263) H51B(0.4256)
 H51C(0.3913) H2A(0.5141) H3A(0.4608) H6(0.4913) H3(0.5179) H5A(0.4785)
 H5(0.5459) H6A(0.5306) H2(0.4644)
;
_olex2_submission_special_instructions 'No special instructions were received'