Zinc(II) and nickel(II) complexes of 3,5-dimethyl-1-(pyridin-2-yl)-1H-pyrazole: relationship between fluorescence and crystal packing
Małecka, Magdalena; Kusz, Joachim; Mayer, Peter; Sobiesiak, Marta; Budzisz, Elzbieta; Acta Crystallographica Section C Structural Chemistry 77 (2021) –; doi:10.1107/S2053229621005374

data_2022390
_publ_section_title
;
 Zinc(II) and nickel(II) complexes of
 3,5-dimethyl-1-(pyridin-2-yl)-1H-pyrazole: relationship between
 fluorescence and crystal packing
;
_journal_coeditor_code           WP3016
_journal_issue                   7
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229621005374
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ni Cl (C10 H11 N3)2 (H2 O)] Cl, H2 O'
_chemical_formula_moiety         'C20 H24 Cl N6 Ni O +, Cl -, H2 O'
_chemical_formula_sum            'C20 H26 Cl2 N6 Ni O2'
_chemical_formula_weight         512.08
_chemical_name_systematic
'Aquachloridobis[3,5-dimethyl-1-(pyridin-2-yl-\k<i>N</i>)-1<i>H</i>-pyrazole-\k<i>N</i>^2^]nickel(II) chloride monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_code                Ni_C10H22N3_Cl_H2O_to071_budzisz
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 100.981(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2306(11)
_cell_length_b                   13.2638(10)
_cell_length_c                   14.0560(14)
_cell_measurement_reflns_used    1291
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.5890
_cell_measurement_theta_min      4.3620
_cell_volume                     2238.5(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008).
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7459
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         4.240
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       rod
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                2776
_reflns_number_total             4070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wp3016sup1.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022390
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.956
_shelx_hkl_checksum              75383
_shelx_res_checksum              72509
_shelxl_version_number           2018/3
_cod_database_fobs_code 2022390