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_7223766
_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         'C14 H7 N O5'
_chemical_formula_sum            'C14 H7 N O5'
_chemical_formula_weight         269.21
_chemical_name_systematic        1-Hyrdoxy-4-nitiroanthraquinone
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 89.137(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3423(2)
_cell_length_b                   10.0879(2)
_cell_length_c                   14.4961(3)
_cell_measurement_reflns_used    12235
_cell_measurement_temperature    120
_cell_measurement_theta_max      71.1520
_cell_measurement_theta_min      5.3160
_cell_volume                     1073.58(4)
_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      293.15
_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   -4.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 26

  2 omega  -69.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 35

  3 omega   36.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -180.0000 32

  4 omega  -85.00  -26.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000    0.0000 59

  5 omega    8.00  120.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   19.0000 -120.0000 112

  6 omega  128.00  173.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   30.0000 45

  7 omega   92.00  177.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000  -60.0000 85

  8 omega   37.00   71.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 34

  9 omega   70.00  101.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  120.0000 31

 10 omega   37.00   66.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000  120.0000 29

 11 omega   40.00   90.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   90.0000 50

 12 omega   43.00   76.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   90.0000 33

 13 omega   39.00   72.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 33

 14 omega   36.00   61.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  -60.0000 25

 15 omega   32.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -60.0000 46

 16 omega  -22.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 91

 17 omega -125.00  -77.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500 -153.0000  132.0000 48

 18 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000    0.0000 103

 19 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  -90.0000 103

 20 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000   90.0000 103

 21 omega -148.00 -100.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -91.0000   30.0000 48

 22 omega   39.00   83.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 44

 23 omega   37.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000   90.0000 141

 24 omega   37.00  149.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -120.0000 112

 25 omega   39.00   83.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  150.0000 44

 26 omega   35.00   72.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 37

 27 omega   82.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   37.0000  150.0000 96

 28 omega   86.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -120.0000 92

 29 omega  -27.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  -90.0000 100

 30 omega  -25.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 69

 31 omega -125.00  -77.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500 -153.0000 -173.0000 48

 32 omega -126.00  -23.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -180.0000 103

 33 omega   33.00  124.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000   60.0000 91

 34 omega  -18.00   85.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -99.0000  120.0000 103

 35 omega -146.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -77.0000  -30.0000 103

 36 omega -145.00  -46.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -73.0000 -108.8823 99

 37 omega -146.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -77.0000  150.0000 103

 38 omega   37.00   71.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 34

 39 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -180.0000 100

 40 omega   85.00  177.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000   90.0000 92

 41 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -30.0000 100

 42 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -90.0000 100

 43 omega   32.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000    0.0000 46

 44 omega  -69.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 91

 45 omega -122.00  -29.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  141.0000  -88.0000 93

 46 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -150.0000 103

 47 omega   73.00  127.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -30.0000 54

 48 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  -30.0000 103

 49 omega -146.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -77.0000   30.0000 103

 50 omega -146.00  -42.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -79.0000   86.4654 104

 51 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000   30.0000 100

 52 omega   35.00   72.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 37

 53 omega   37.00  149.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 112

 54 omega   37.00  149.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000 -180.0000 112

 55 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000    0.0000 100

 56 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  150.0000 100

 57 omega  -73.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000 -120.0000 100

 58 omega  -71.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -150.0000 103

 59 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  -60.0000 103

 60 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  150.0000 103

 61 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000   60.0000 103

 62 omega   23.00  126.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -120.0000 103

 63 omega -146.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -77.0000 -150.0000 103

 64 omega -146.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -77.0000  -60.0000 103

 65 omega -146.00  -42.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -75.0000  -79.0000  111.0374 104

 66 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -60.0000 100

 67 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  120.0000 100

 68 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000   60.0000 100

 69 omega   78.00  178.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000 -120.0000 100

 70 omega   85.00  177.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      109.5000   63.0000 -150.0000 92
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0144582000
_diffrn_orient_matrix_UB_12      -0.1347774000
_diffrn_orient_matrix_UB_13      0.0493371000
_diffrn_orient_matrix_UB_21      -0.0189044000
_diffrn_orient_matrix_UB_22      0.0700905000
_diffrn_orient_matrix_UB_23      0.0940754000
_diffrn_orient_matrix_UB_31      -0.2084915000
_diffrn_orient_matrix_UB_32      -0.0156101000
_diffrn_orient_matrix_UB_33      -0.0035112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23531
_diffrn_reflns_theta_full        71.21
_diffrn_reflns_theta_max         71.21
_diffrn_reflns_theta_min         5.34
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.738
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.4737
_exptl_crystal_size_mid          0.1084
_exptl_crystal_size_min          0.0722
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.084
_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     181
_refine_ls_number_reflns         2061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0964P)^2^+0.2599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                1876
_reflns_number_total             2061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01658d2.cif
_cod_data_source_block           st298-b-cu-120k_abs
_cod_database_code               7223766
_chemical_oxdiff_formula         'C14 O5 N H5'
_reflns_odcompleteness_completeness 93.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Riding coordinates:
 O5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'