DOSY NMR, X-ray Structural and Ion-Mobility Mass Spectrometric Studies on Electron-Deficient and Electron-Rich M6L4 Coordination Cages.
Bonakdarzadeh, Pia; Topić, Filip; Kalenius, Elina; Bhowmik, Sandip; Sato, Sota; Groessl, Michael; Knochenmuss, Richard; Rissanen, Kari; Inorganic chemistry 54 (2015) 6055–6061; doi:10.1021/acs.inorgchem.5b01082

data_4343105
_publ_section_title
;
 DOSY NMR, X-ray Structural and Ion-Mobility Mass Spectrometric Studies on
 Electron-Deficient and Electron-Rich M6L4 Coordination Cages.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6055
_journal_page_last               6061
_journal_paper_doi               10.1021/acs.inorgchem.5b01082
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '0.5(C H Cl3), C27 H12 F3 N3'
_chemical_formula_sum            'C27.5 H12.5 Cl1.5 F3 N3'
_chemical_formula_weight         495.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2015-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9012(7)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.5580(1)
_cell_length_b                   20.4595(2)
_cell_length_c                   33.6987(2)
_cell_measurement_reflns_used    14339
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      73.6100
_cell_measurement_theta_min      3.9880
_cell_volume                     9235.10(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega -115.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -57.0000 -120.0000 98

  2 omega   25.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9013 -125.0000    0.0000 73

  3 omega   33.00  107.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  120.0000 74

  4 omega   47.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000  -60.0000 44

  5 omega   24.00  103.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000    0.0000 79

  6 omega   85.00  178.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   45.0000  -30.0000 93

  7 omega   35.00  131.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -61.0000 -180.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0246934000
_diffrn_orient_matrix_UB_12      -0.0289205000
_diffrn_orient_matrix_UB_13      0.0425905000
_diffrn_orient_matrix_UB_21      -0.0127284000
_diffrn_orient_matrix_UB_22      0.0680289000
_diffrn_orient_matrix_UB_23      0.0180868000
_diffrn_orient_matrix_UB_31      -0.1116442000
_diffrn_orient_matrix_UB_32      -0.0142138000
_diffrn_orient_matrix_UB_33      -0.0000149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            30072
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.247
_diffrn_reflns_theta_min         3.996
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.400
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       prism
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         16354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+2.3278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14201
_reflns_number_total             16354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01082_si_002.cif
_cod_data_source_block           L1
_cod_depositor_comments
'Adding full bibliography for 4343103--4343105.cif.'
_cod_original_cell_volume        9235.1(1)
_cod_database_code               4343105
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C03(H03), C03Q(H03Q)
2.b Aromatic/amide H refined with riding coordinates:
 C01Q(H01Q), C01R(H01R), C01X(H01X), C01Y(H01Y), C023(H023), C025(H025),
 C027(H027), C02B(H02B), C02D(H02D), C02K(H02K), C02L(H02L), C02M(H02M),
 C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C02T(H02T),
 C02V(H02V), C02W(H02W), C02X(H02X), C02Y(H02Y), C02Z(H02Z), C030(H030),
 C032(H032), C035(H035), C037(H037), C038(H038), C039(H039), C03A(H03A),
 C03C(H03C), C03D(H03D), C03E(H03E), C03F(H03F), C03G(H03G), C03I(H03I),
 C03J(H03J), C03K(H03K), C03L(H03L), C03M(H03M), C03N(H03N), C03P(H03P),
 C03R(H03R), C03S(H03S), C03T(H03T), C03U(H03U), C03V(H03V), C03W(H03W)
;
_olex2_submission_special_instructions 'No special instructions were received'