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_7028499
_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
'C69 H96 N6 Ni3 O3 S3  , 1.5(C2 H6 O) , 1.5(C H2 Cl2)'
_chemical_formula_sum            'C73.5 H108 Cl3 N6 Ni3 O4.5 S3'
_chemical_formula_weight         1526.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.884(4)
_cell_angle_beta                 83.960(4)
_cell_angle_gamma                88.575(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1982(12)
_cell_length_b                   13.1994(15)
_cell_length_c                   24.094(3)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     3854.3(8)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0662
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37519
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.9535
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Originally approx 1.5CH2Cl2 and 1.5 EtOH were found but
did not refine properly due to severe disorder.
The electron count found by SQUEEZE after removal of the solvent
corresponds quite closely to 1.5CH2Cl2 und 1.5 EtOH which are now
included in the sum formula and derived quantities.
;
_refine_diff_density_max         1.595
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                8502
_reflns_number_total             13195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53457j.txt
_cod_data_source_block           g2005
_cod_original_cell_volume        3854.4(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C73.50 H108 Cl3 N6 Ni3 O4.50 S3'
_cod_database_code               7028499