Dual modes of binding on the hexafluorosilicate anion by a C3v symmetric flexible tripodal amide ligand in solid state
Basu, Arghya; Chutia, Romen; Das, Gopal; CrystEngComm 16 (2014) 4886–; doi:10.1039/c4ce00529e

data_7216419
_publ_section_title
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 Dual modes of binding on the hexafluorosilicate anion by a C3v symmetric
 flexible tripodal amide ligand in solid state
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_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4886
_journal_paper_doi               10.1039/c4ce00529e
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C96 H102 F6 N16 O30 Si'
_chemical_formula_weight         2102.03
_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                108.655(2)
_cell_angle_beta                 105.033(2)
_cell_angle_gamma                92.632(2)
_cell_formula_units_Z            1
_cell_length_a                   13.1197(5)
_cell_length_b                   13.1321(6)
_cell_length_c                   15.7929(6)
_cell_measurement_reflns_used    7460
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.17
_cell_measurement_theta_min      2.15
_cell_volume                     2464.94(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1291
_diffrn_reflns_av_sigmaI/netI    0.1083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30365
_diffrn_reflns_theta_full        27.78
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             1098.0
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0011(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         11455
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1831
_reflns_number_gt                9244
_reflns_number_total             11455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00529e2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/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_cell_volume        2464.94(17)
_cod_database_code               7216419