Three Metal Complexes Derived from 3-Methyl-1H-Pyrazole-4-Carboxylic Acid: Synthesis, Crystal Structures, Luminescence and Electrocatalytic Properties
Liu, Qi; Liu, Jing; Cheng, Mei-Ling; Yu, Lili; Chen, Sheng-Chun; Shao, Yongliang; Zhai, Changwei; Yin, Fengxiang; RSC Adv.  (2016) –; doi:10.1039/C6RA10989F

data_7225337
_publ_section_title
;
 Three Metal Complexes Derived from 3-Methyl-1H-Pyrazole-4-Carboxylic
 Acid: Synthesis, Crystal Structures, Luminescence and Electrocatalytic
 Properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA10989F
_journal_year                    2016
_chemical_formula_moiety         '0.5(C40 H48 Cd6 Cl4 N16 O20), 2(H2 O)'
_chemical_formula_sum            'C20 H28 Cd3 Cl2 N8 O12'
_chemical_formula_weight         980.60
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2013-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2015-12-10 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.760(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.587(2)
_cell_length_b                   14.232(3)
_cell_length_c                   12.454(3)
_cell_measurement_reflns_used    2976
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.055
_cell_measurement_theta_min      2.407
_cell_volume                     1643.2(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10069
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.650
_diffrn_reflns_theta_min         2.215
_exptl_absorpt_coefficient_mu    2.153
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.184
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3665
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0595P)^2^+4.3678P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2654
_reflns_number_total             3665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra10989f2.cif
_cod_data_source_block           t
_cod_original_cell_volume        1643.1(6)
_cod_database_code               7225337
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6A = O6-H6B
 0.82 with sigma of 0.01
 H6A-H6B
 1.46 with sigma of 0.01
3.a Riding coordinates:
 N2(H2), N4(H4), O6(H6A,H6B)
3.b Rotating group:
 O5(H5A,H5B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8)
3.d Idealised Me refined as rotating group:
 C5(H5C,H5D,H5E), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              68805