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_7028500
_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_absolute_configuration ad
_chemical_formula_moiety         'C69 H96 N6 O3 S3 Ni3 , C H2 Cl2 , H2 O'
_chemical_formula_sum            'C70 H100 Cl2 N6 Ni3 O4 S3'
_chemical_formula_weight         1432.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_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            24
_cell_length_a                   24.7936(5)
_cell_length_b                   24.7936(5)
_cell_length_c                   89.645(3)
_cell_measurement_reflns_used    8105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      10.80
_cell_volume                     47724(2)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'X8 PROSPECTOR ULTRA'
_diffrn_measurement_device_type  'three circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'QuazarTM Montel Multilayer optics'
_diffrn_radiation_source         'I\mS Incoatec Microfocus Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1052
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       105
_diffrn_reflns_limit_l_min       -106
_diffrn_reflns_number            79261
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         10.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.529
_exptl_absorpt_correction_T_max  0.8840
_exptl_absorpt_correction_T_min  0.6878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             18240
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;

 Approx. 0.56 CH2CL2 and 0.31 H2O molecules per complex can be found 
 disordered and refined. Together with the electron density found by
 Squeeze 1 CH2CL2 and 1 H2O molecule can be attributed to each complex 
 molecule and is therefore included in the sum formula ad derived quantities.
;
_refine_diff_density_max         1.858
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2074
_refine_ls_number_reflns         34119
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                25902
_reflns_number_total             34119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53457j.txt
_cod_data_source_block           g2025
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7028500