Coordination environments and π-conjugation in dense lithium coordination polymers
Tominaka, Satoshi; Yeung, Hamish H.-M.; Henke, Sebastian; Cheetham, Anthony K.; CrystEngComm 18 (2016) 398–; doi:10.1039/C5CE01658D

data_7223765
_publ_section_title
;
 Coordination environments and \p-conjugation in dense lithium
 coordination polymers
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              398
_journal_paper_doi               10.1039/C5CE01658D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '2(C7 H7 Li O4), H2 O'
_chemical_formula_sum            'C14 H16 Li2 O9'
_chemical_formula_weight         342.15
_chemical_name_systematic        '1,5-dihydroxyanthraquinone lithium salt'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-17 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                97.619(4)
_cell_angle_beta                 91.892(4)
_cell_angle_gamma                108.338(5)
_cell_formula_units_Z            2
_cell_length_a                   5.0112(2)
_cell_length_b                   7.5031(4)
_cell_length_c                   21.0358(8)
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    121(3)
_cell_measurement_theta_max      62.8550
_cell_measurement_theta_min      4.2460
_cell_volume                     741.79(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      121(3)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -90.00  -17.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -      -34.0930  124.0000  -36.0000 73

  2 omega   38.00  102.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930   57.0000 -120.0000 64

  3 omega   38.00  107.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930  178.0000  -90.0000 69

  4 omega   14.00   96.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930   57.0000  120.0000 82

  5 omega  -31.00   49.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930  -37.0000  -60.0000 80

  6 omega   25.00  126.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -91.0000  -97.6489 101

  7 omega   74.00  101.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000  128.6218 27

  8 omega   20.00   47.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000   36.9144 27

  9 omega   18.00   44.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -17.0000  -18.3117 26

 10 omega   20.00  111.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -84.0000   62.1541 91

 11 omega   56.00  109.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -17.0000  -18.3117 53

 12 omega   54.00  101.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   22.0000   -1.0367 47

 13 omega  108.00  159.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   22.0000   -1.0367 51

 14 omega   59.00  121.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  178.0000   90.0000 62

 15 omega   21.00   47.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000  128.6218 26

 16 omega   42.00   89.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000 -111.0000 -120.0000 47

 17 omega   21.00   68.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -180.0000 47

 18 omega   71.00   97.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000   97.6845 26

 19 omega  111.00  137.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  111.0000   60.0000 26

 20 omega   26.00   74.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  150.0000 48

 21 omega   33.00   76.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000 -120.0000 43

 22 omega   18.00   66.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000   90.0000 48

 23 omega   18.00  123.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000    0.0000  150.0000 105

 24 omega  133.00  159.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000    0.0000  150.0000 26

 25 omega   25.00   74.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -60.0000 49

 26 omega   23.00   60.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000 -111.0000  -90.0000 37

 27 omega   42.00   79.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -77.0000  -90.0000 37

 28 omega   20.00   55.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000 -111.0000 -180.0000 35

 29 omega   76.00  101.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -61.0000   90.0000 25

 30 omega   27.00   54.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000   60.0000 27

 31 omega   23.00   51.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -61.0000   90.0000 28

 32 omega   24.00   49.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -150.0000 25

 33 omega   19.00   44.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -15.0000  120.0000 25

 34 omega  112.00  143.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -15.0000  120.0000 31

 35 omega   29.00   54.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000   97.6845 25

 36 omega   29.00   55.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000   90.0000 26

 37 omega   75.00  105.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000   36.9144 30

 38 omega  137.00  162.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  111.0000  -90.0000 25

 39 omega   42.00   98.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  -24.9581 56

 40 omega   98.00  123.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  178.0000 -150.0000 25

 41 omega   71.00  100.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000 -136.7190 29

 42 omega  -54.00   35.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -      -34.0930   57.0000  -30.0000 89

 43 omega -110.00  -57.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -      -34.0930 -178.0000  120.0000 53

 44 omega    4.00  104.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930   77.0000 -180.0000 100

 45 omega   14.00  103.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930   57.0000    0.0000 89

 46 omega   14.00  103.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930   57.0000   60.0000 89

 47 omega   35.00  110.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930  178.0000  150.0000 75

 48 omega    4.00  104.00   1.0000    3.0900
omega____ theta____ kappa____ phi______ frames
    -       34.0930   77.0000  -90.0000 100

 49 omega -134.00  -34.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000    0.0000 100

 50 omega -134.00  -34.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000 -120.0000 100

 51 omega -134.00  -34.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000 -180.0000 100

 52 omega -134.00  -35.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -76.0000   77.3344 99

 53 omega -134.00  -34.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -77.0000  -60.0000 100

 54 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000 -150.0000 101

 55 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000   90.0000 101

 56 omega   60.00  137.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000 -180.0000 77

 57 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  -30.0000 101

 58 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000   30.0000 101

 59 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000   60.0000 101

 60 omega   67.00  162.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000  -90.0000 95

 61 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  -60.0000 101

 62 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000    0.0000 101

 63 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  120.0000 101

 64 omega   60.00  161.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  -90.0000 101

 65 omega   61.00  163.00   1.0000    8.6300
omega____ theta____ kappa____ phi______ frames
    -       90.5000   30.0000 -150.0000 102
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.3044655000
_diffrn_orient_matrix_UB_12      -0.0349541000
_diffrn_orient_matrix_UB_13      0.0190334000
_diffrn_orient_matrix_UB_21      -0.1102161000
_diffrn_orient_matrix_UB_22      -0.0609734000
_diffrn_orient_matrix_UB_23      -0.0713845000
_diffrn_orient_matrix_UB_31      -0.0266829000
_diffrn_orient_matrix_UB_32      -0.2072117000
_diffrn_orient_matrix_UB_33      0.0059994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14922
_diffrn_reflns_theta_full        63.05
_diffrn_reflns_theta_max         63.05
_diffrn_reflns_theta_min         4.25
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.4764
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.0183
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.2080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                2115
_reflns_number_total             2377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01658d2.cif
_cod_data_source_block           st237_cu_st_re_abs2
_cod_database_code               7223765
_chemical_oxdiff_formula         'C14 H16 Li2 O9'
_reflns_odcompleteness_completeness 97.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O3(H3A,H3B), O4(H4A,H4B), O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'