A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni(II)3 complexes.
Feldscher, Bastian; Theil, Hubert; Stammler, Anja; Bögge, Hartmut; Glaser, Thorsten; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4102–4114; doi:10.1039/c3dt53457j

data_7028498
_publ_section_title
;
 A streamlined synthesis of extended thiophloroglucinol ligands and their
 trinuclear Ni(II)3 complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4102
_journal_page_last               4114
_journal_paper_doi               10.1039/c3dt53457j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C48 H54 N6 Ni3 O3 S3 , 2(C7 H8)'
_chemical_formula_sum            'C62 H70 N6 Ni3 O3 S3'
_chemical_formula_weight         1219.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.4863(17)
_cell_length_b                   21.4863(17)
_cell_length_c                   27.386(3)
_cell_measurement_reflns_used    6728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.31
_cell_volume                     10949.2(17)
_computing_cell_refinement       'APEX2  (Bruker AXS, 2009)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker KAPPA APEX II'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38677
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.8858
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3540
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
 
 Originally one toluene molecule was found disordered in the region of 
 each void, but it could not properly be refined  and was therefore
 removed from the coordinate set. The resulting void was then
 treated with "SQUEEZE". The found electron count can be attributed to ca 
 two toluene molecules. These were included in the given sum formula and thus
 contribute to derived quantities like mu rho etc.

;
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4282
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.2093
_reflns_number_gt                2516
_reflns_number_total             4282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53457j.txt
_cod_data_source_block           g1905
_cod_original_cell_volume        10949.2(16)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7028498