Thioether-terminated nickel(ii) coordination clusters with {Ni6} horseshoe- and {Ni8} rollercoaster-shaped cores
Schmitz, Sebastian; van Leusen, Jan; Ellern, Arkady; Kögerler, Paul; Monakhov, Kirill Yu.; Inorganic Chemistry Frontiers 3 (2016) 523–; doi:10.1039/C5QI00278H

data_4349092
_publ_section_title
;
 Thioether-terminated nickel(ii) coordination clusters with {Ni6}
 horseshoe- and {Ni8} rollercoaster-shaped cores
;
_journal_issue                   4
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              523
_journal_paper_doi               10.1039/C5QI00278H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety
;
C92 H86 N12 Ni8 O20 S4, 2(C7 H5 N), 2(N O3), 11(C2 H3 N)  
;
_chemical_formula_sum            'C114 H119 N25 Ni8 O26 S4'
_chemical_formula_weight         2853.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-01 deposited with the CCDC.
2016-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.191(8)
_cell_angle_beta                 95.030(9)
_cell_angle_gamma                113.761(8)
_cell_formula_units_Z            2
_cell_length_a                   17.742(8)
_cell_length_b                   18.183(8)
_cell_length_c                   20.695(9)
_cell_measurement_reflns_used    3890
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      2.24
_cell_volume                     6081(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2004
_diffrn_reflns_av_unetI/netI     0.2452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.892
_diffrn_reflns_theta_min         1.260
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.166
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1437
_refine_ls_number_reflns         25374
_refine_ls_number_restraints     797
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1993
_refine_ls_R_factor_gt           0.1190
_refine_ls_shift/su_max          0.134
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1745P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2939
_refine_ls_wR_factor_ref         0.3570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11951
_reflns_number_total             25374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00278h2.cif
_cod_data_source_block           mon006_sq
_cod_database_code               4349092
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              36166
_shelx_hkl_checksum              60478
_shelx_fab_checksum              73801