Ligand Effects on the Structure, Mixed-valence Sites and Magnetic Properties of Novel Pentanickel String Complexes
Chiu, Cheng-Chang; Lee, Gene-Hsiang; Lin, Tien-Sung; Peng, Shie-Ming; Dalton Transactions  (2019) –; doi:10.1039/C9DT01363F

data_7049991
_publ_section_title
;
 Ligand Effects on the Structure, Mixed-valence Sites and Magnetic
 Properties of Novel Pentanickel String Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT01363F
_journal_year                    2019
_chemical_formula_sum            'C109.5 H87 Cl11 F6 N20 Ni5 O8 P S4'
_chemical_formula_weight         2767.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-15 deposited with the CCDC.    2019-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                73.6370(14)
_cell_angle_beta                 76.3465(16)
_cell_angle_gamma                76.0990(18)
_cell_formula_units_Z            2
_cell_length_a                   16.4220(7)
_cell_length_b                   16.8719(8)
_cell_length_c                   22.4552(10)
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.51
_cell_volume                     5699.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47815
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.080
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       plate
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.691
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1554
_refine_ls_number_reflns         26098
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+21.5144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19485
_reflns_number_total             26098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01363f2.cif
_cod_data_source_block           ic18269
_cod_original_formula_sum        'C109.50 H87 Cl11 F6 N20 Ni5 O8 P S4'
_cod_database_code               7049991
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.747
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              57632