Synthesis and Solid-State Characterization of Self-Assembled Macrocyclic Molecular Rotors of Bis(dithiocarbamate) Ligands with Diorganotin(IV)
Torres-Huerta, Aarón; Rodríguez-Molina, Braulio; Höpfl, Herbert; Garcia-Garibay, Miguel A.; Organometallics 33 (2014) 354–; doi:10.1021/om401094d

data_4082561
_publ_section_title
;
 Synthesis and Solid-State Characterization of Self-Assembled Macrocyclic
 Molecular Rotors of Bis(dithiocarbamate) Ligands with Diorganotin(IV)
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              354
_journal_paper_doi               10.1021/om401094d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C52 H56 N4 S8 Sn2, 2(C H2 CL2)'
_chemical_formula_sum            'C54 H60 Cl4 N4 S8 Sn2'
_chemical_formula_weight         1400.72
_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                110.697(2)
_cell_angle_beta                 99.399(2)
_cell_angle_gamma                90.789(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4506(16)
_cell_length_b                   10.5448(16)
_cell_length_c                   14.799(2)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      3.87
_cell_volume                     1500.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0208
_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       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21235
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.80
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  0.8787
_exptl_absorpt_correction_T_min  0.7171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8529
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0398P)^2^+1.2158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                7644
_reflns_number_total             8529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401094d_si_002.cif
_cod_data_source_block           gg2211s1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082561