Crown ether alkali metal TCNQ complexes revisited – the impact of smaller cation complexes on their solid-state architecture and properties
Yan, Bingjia; Horton, Peter N.; Russell, Andrea E.; Wedge, Christopher J.; Weston, Simon C.; Grossel, Martin C.; CrystEngComm 21 (2019) 3273–; doi:10.1039/C9CE00234K

data_7232682
_publ_section_title
;
 Crown ether alkali metal TCNQ complexes revisited -- the impact of
 smaller cation complexes on their solid-state architecture and properties
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3273
_journal_paper_doi               10.1039/C9CE00234K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C10 H22 Li O6, 2(C12 H4 N4)'
_chemical_formula_sum            'C34 H30 Li N8 O6'
_chemical_formula_weight         653.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-06 deposited with the CCDC.    2019-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                97.615(5)
_cell_angle_beta                 100.354(5)
_cell_angle_gamma                100.015(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3032(5)
_cell_length_b                   12.4300(7)
_cell_length_c                   16.5807(12)
_cell_measurement_reflns_used    5650
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7790
_cell_measurement_theta_min      2.5010
_cell_volume                     1633.89(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  73.00   1.00   30.00    --  -17.00  72.00  30.00  100
  2  \w    -69.00  22.00   1.00   30.00    --  -17.00 -72.00 -90.00   91
  3  \w    -66.00  22.00   1.00   30.00    --  -17.00 -72.00  90.00   88
  4  \w    -84.00 -21.00   1.00   30.00    --  -17.00   0.00 -90.00   63
  5  \w     -4.00  16.00   1.00   30.00    --  -17.00 -36.00  90.00   20
  6  \w    -27.00  73.00   1.00   30.00    --  -17.00  72.00 -60.00  100
  7  \w    -69.00  22.00   1.00   30.00    --  -17.00 -72.00-180.00   91
  8  \w    -69.00 -48.00   1.00   30.00    --  -17.00 -72.00   0.00   21
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210765000
_diffrn_orient_matrix_UB_12      0.0007140000
_diffrn_orient_matrix_UB_13      -0.0432954000
_diffrn_orient_matrix_UB_21      0.0489160000
_diffrn_orient_matrix_UB_22      0.0543623000
_diffrn_orient_matrix_UB_23      0.0062753000
_diffrn_orient_matrix_UB_31      0.0709051000
_diffrn_orient_matrix_UB_32      -0.0223793000
_diffrn_orient_matrix_UB_33      -0.0057342000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20928
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.688
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plate
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.0767
_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/[\s^2^(Fo^2^)+(0.0683P)^2^+1.7325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4263
_reflns_number_total             7458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00234k2.cif
_cod_data_source_block           3_5LiT2
_cod_depositor_comments
'Adding full bibliography for 7232678--7232682.cif.'
_cod_original_cell_volume        1633.89(18)
_cod_database_code               7232682
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H22 Li O6 (C12H4N4)2'
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.993
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C305(H30I,
 H30J), C306(H30K,H30L), C307(H30M,H30N), C308(H30O,H30P), C309(H30Q,H30R),
 C310(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C105(H105), C106(H106), C202(H202), C203(H203),
 C205(H205), C206(H206)
;
_shelx_res_checksum              57562
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.906
_oxdiff_exptl_absorpt_empirical_full_min 0.580