Bis(2,2':6',2''-terpyridine-κ^3^<i>N</i>,<i>N</i>',<i>N</i>'')nickel(II) bis(perchlorate) hemihydrate
Anderer, Carolin; Näther, Christian; Bensch, Wolfgang; IUCrData 1 (2016) x161009–; doi:10.1107/S2414314616010099

data_1543620
_publ_section_title
;
 Bis(2,2':6',2''-terpyridine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>'')nickel(II)
 bis(perchlorate) hemihydrate
;
_journal_coeditor_code           SU4053
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x161009
_journal_paper_doi               10.1107/S2414314616010099
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '[Ni (C15 H11 N3)2] (Cl O4)2, 0.5H2 O'
_chemical_formula_moiety         'C30 H22 N6 Ni 2+, 2(Cl O4 -), 0.5(H2 O)'
_chemical_formula_sum            'C30 H23 Cl2 N6 Ni O8.5'
_chemical_formula_weight         733.15
_chemical_name_systematic
;
Bis(2,2':6',2''-terpyridine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>'')nickel(II)
bis(perchlorate) hemihydrate
;
_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_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 94.150(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7733(2)
_cell_length_b                   8.8342(2)
_cell_length_c                   39.4158(10)
_cell_measurement_reflns_used    31108
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.590
_cell_measurement_theta_min      1.036
_cell_volume                     3046.92(12)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            31108
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.590
_diffrn_reflns_theta_min         1.036
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.353
_refine_ls_extinction_coef       0.0049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2013 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0634P)^2^+1.5903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                4629
_reflns_number_total             5107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su4053sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1543620.cif.'
_cod_original_formula_sum        'C30 H23 Cl2 N6 Ni O8.50'
_cod_database_code               1543620
_cod_database_fobs_code          1543620
_shelx_hkl_checksum              70138
_shelx_res_checksum              63736
_shelxl_version_number           2.014