#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:09:19 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179525 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/22/4342250.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4342250
loop_
_publ_author_name
'Deshmukh, Mahesh S.'
'Yadav, Ashok'
'Pant, Rakesh'
'Boomishankar, Ramamoorthy'
_publ_section_title
;
 Thermochromic and Mechanochromic Luminescence Umpolung in Isostructural
 Metal-Organic Frameworks Based on Cu6I6 Clusters.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1337
_journal_page_last               1345
_journal_paper_doi               10.1021/ic502207f
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C16 H15 N3 Si'
_chemical_formula_weight         277.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.664(4)
_cell_length_b                   13.664(4)
_cell_length_c                   13.849(4)
_cell_measurement_reflns_used    724
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      2.98
_cell_volume                     2239.3(11)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex Duo'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4888
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_min         2.264
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       squar
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1440P)²+8.6773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.2485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                905
_reflns_number_total             1248
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic502207f_si_009.cif
_cod_data_source_block           TRI1
_cod_depositor_comments
'Adding full bibliography for 4342249--4342255.cif.'
_cod_original_cell_volume        2239.2(15)
_cod_database_code               4342250
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Si1 Si 1.0000 1.0000 0.24266(9) 0.0210(5) Uani 1 3 d S T P
C1 C 1.0000 1.0000 0.3772(4) 0.0333(13) Uani 1 3 d S T P
H1A H 1.0656 1.0694 0.4007 0.050 Uiso 0.3333 1 calc R U P
H1B H 1.0038 0.9344 0.4007 0.050 Uiso 0.3333 1 calc R U P
H1C H 0.9306 0.9962 0.4007 0.050 Uiso 0.3333 1 calc R U P
C11 C 0.8667(3) 0.8768(3) 0.1954(2) 0.0219(7) Uani 1 1 d . . .
C12 C 0.8615(3) 0.8143(3) 0.1126(2) 0.0277(7) Uani 1 1 d . . .
H12 H 0.9289 0.8311 0.0793 0.033 Uiso 1 1 calc R U .
N13 N 0.7592(3) 0.7292(3) 0.0801(2) 0.0432(9) Uani 1 1 d . . .
C14 C 0.6616(3) 0.7055(3) 0.1311(3) 0.0322(8) Uani 1 1 d . . .
H14 H 0.5907 0.6475 0.1077 0.039 Uiso 1 1 calc R U .
C15 C 0.6634(3) 0.7611(3) 0.2118(2) 0.0265(7) Uani 1 1 d . . .
H15 H 0.5963 0.7421 0.2466 0.032 Uiso 1 1 calc R U .
C16 C 0.7642(3) 0.8442(3) 0.2405(2) 0.0288(8) Uani 1 1 d . . .
H16 H 0.7659 0.8847 0.2969 0.035 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Si1 C11 110.45(9) . .
C1 Si1 C11 110.45(9) . 3_675
C11 Si1 C11 108.47(10) . 3_675
C1 Si1 C11 110.45(9) . 2_765
C11 Si1 C11 108.47(10) . 2_765
C11 Si1 C11 108.47(10) 3_675 2_765
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C16 C11 C12 115.7(3) . .
C16 C11 Si1 120.1(2) . .
C12 C11 Si1 124.1(2) . .
N13 C12 C11 120.2(3) . .
N13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C12 N13 C14 118.7(3) . .
C15 C14 N13 122.9(3) . .
C15 C14 H14 118.5 . .
N13 C14 H14 118.5 . .
C16 C15 C14 116.7(3) . .
C16 C15 H15 121.7 . .
C14 C15 H15 121.7 . .
C15 C16 C11 125.8(3) . .
C15 C16 H16 117.1 . .
C11 C16 H16 117.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.863(5) .
Si1 C11 1.874(3) .
Si1 C11 1.874(3) 3_675
Si1 C11 1.874(3) 2_765
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C11 C16 1.389(4) .
C11 C12 1.409(4) .
C12 N13 1.372(5) .
C12 H12 0.9500 .
N13 C14 1.397(5) .
C14 C15 1.345(5) .
C14 H14 0.9500 .
C15 C16 1.334(5) .
C15 H15 0.9500 .
C16 H16 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C1 Si1 C11 C16 39.5(3) .
C11 Si1 C11 C16 -81.7(3) 3_675
C11 Si1 C11 C16 160.7(3) 2_765
C1 Si1 C11 C12 -142.7(2) .
C11 Si1 C11 C12 96.1(2) 3_675
C11 Si1 C11 C12 -21.5(3) 2_765
C16 C11 C12 N13 1.5(5) .
Si1 C11 C12 N13 -176.4(3) .
C11 C12 N13 C14 -0.7(5) .
C12 N13 C14 C15 -1.2(5) .
N13 C14 C15 C16 2.0(5) .
C14 C15 C16 C11 -1.1(5) .
C12 C11 C16 C15 -0.7(5) .
Si1 C11 C16 C15 177.3(3) .
