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_4349095
_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
;
C78 H85 N6 Ni6 O20 S3, 2(C H4 O), Cl
;
_chemical_formula_sum            'C80 H93 Cl N6 Ni6 O22 S3'
_chemical_formula_weight         1974.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 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
_cell_angle_beta                 97.636(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7711(17)
_cell_length_b                   21.197(3)
_cell_length_c                   15.366(2)
_cell_measurement_reflns_used    4853
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      23.41
_cell_measurement_theta_min      2.17
_cell_volume                     4122.8(10)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2013)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2013)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.516
_diffrn_reflns_theta_min         0.961
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0377P)^2^+3.9945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6612
_reflns_number_total             8544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00278h2.cif
_cod_data_source_block           Mon005
_cod_original_cell_volume        4122.9(9)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4349095
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              99030
_shelx_hkl_checksum              24934