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_7028497
_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
'C30 H54 N9 Ni3 S3, 3(B C24 H20) , 3( C3 H6 O)'
_chemical_formula_sum            'C111 H132 B3 N9 Ni3 O3 S3'
_chemical_formula_weight         1945.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.034(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7065(11)
_cell_length_b                   33.162(2)
_cell_length_c                   17.0365(10)
_cell_measurement_reflns_used    9265
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.00
_cell_measurement_theta_min      2.50
_cell_volume                     10003.5(10)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker X8 Prospector Ultra'
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            89035
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_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    1.673
_exptl_absorpt_correction_T_max  0.8143
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
 In preliminary refinements 3 acetone molecules were found strongly 
 disordered over approx 5 positions. This is in good aggreement 
 with the number of electrons and the corresponding void volume found
 by PLATON/SQUEEZE. 
 The acetone molecules are thus included in the chemical formulas
 and quantities derived from them.
;
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         18244
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+8.7430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                15267
_reflns_number_total             18244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53457j.txt
_cod_data_source_block           g1889
_cod_original_cell_volume        10003.7(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7028497