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_7225338
_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         'C10 H18 Cd N4 O8'
_chemical_formula_sum            'C10 H18 Cd N4 O8'
_chemical_formula_weight         434.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-17
_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                111.267(3)
_cell_angle_beta                 109.883(3)
_cell_angle_gamma                91.968(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2694(10)
_cell_length_b                   7.2818(11)
_cell_length_c                   8.2989(12)
_cell_measurement_reflns_used    1369
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.85
_cell_volume                     378.69(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2168
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.7070
_exptl_absorpt_correction_T_min  0.6470
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             218
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1369
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.2865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                1355
_reflns_number_total             1369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra10989f2.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        378.69(9)
_cod_database_code               7225338
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H3B-O3 = H3A-O3
 0.86 with sigma of 0.02
 H3A-H3B
 1.46 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Rotating group:
 O4(H4D,H4E)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1)
4.c Idealised Me refined as rotating group:
 C4(H4B,H4C,H4A)
;