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_4349094
_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
;
C42 H36 N4 Ni O6, 2(N O3), 4(C H4 O) 
;
_chemical_formula_sum            'C44 H44 N6 Ni O14'
_chemical_formula_weight         939.56
_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
_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                 101.750(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   13.6631(8)
_cell_length_b                   55.396(3)
_cell_length_c                   17.4219(10)
_cell_measurement_reflns_used    6002
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.92
_cell_measurement_theta_min      2.19
_cell_volume                     12910.0(13)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1510
_diffrn_reflns_av_unetI/netI     0.1080
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.826
_diffrn_reflns_theta_max         20.826
_diffrn_reflns_theta_min         0.735
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             5880
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1774
_refine_ls_number_reflns         13531
_refine_ls_number_restraints     1614
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.1170
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+216.9637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2855
_refine_ls_wR_factor_ref         0.3020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10525
_reflns_number_total             13531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00278h2.cif
_cod_data_source_block           mon010_sq
_cod_original_cell_volume        12910.1(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349094
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              34444
_shelx_hkl_checksum              84285
_shelx_fab_checksum              13465