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_7223763
_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_absolute_configuration unk
_chemical_formula_moiety         'C14 H8 Li N O6'
_chemical_formula_sum            'C14 H8 Li N O6'
_chemical_formula_weight         293.16
_chemical_name_systematic        'Lithium 1-hydroxy-4-nitroanthraquinone'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8535(3)
_cell_length_b                   13.0952(10)
_cell_length_c                   18.9644(12)
_cell_measurement_reflns_used    1526
_cell_measurement_temperature    120
_cell_measurement_theta_max      61.1950
_cell_measurement_theta_min      4.1025
_cell_volume                     1205.33(14)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega -110.00  -62.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -      -31.9956  178.0000 -120.0000 48

  2 omega -110.00  -81.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -      -31.9956 -178.0000   90.0000 29

  3 omega   57.00   87.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -       31.9956   57.0000   30.0000 30

  4 omega   -6.00   52.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -       31.9956  -57.0000   60.0000 58

  5 omega -133.00 -105.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -      -75.0000 -111.0000  120.0000 28

  6 omega   19.00   61.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409  -30.0000  -30.0000 42

  7 omega   97.00  124.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409  111.0000   90.0000 27

  8 omega   53.00   84.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409  -94.0000  -90.0000 31

  9 omega   17.00   49.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409  -94.0000  -90.0000 32

 10 omega   22.00  110.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409  -61.0000   30.0000 88

 11 omega   45.00   77.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409  -94.0000 -150.0000 32

 12 omega   10.00  101.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -       31.9956   57.0000 -150.0000 91

 13 omega    5.00  105.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -       31.9956   37.0000  120.0000 100

 14 omega   10.00  101.00   1.0000    5.3400
omega____ theta____ kappa____ phi______ frames
    -       31.9956   57.0000  -30.0000 91

 15 omega   58.00  100.00   1.0000  186.5600
omega____ theta____ kappa____ phi______ frames
    -       89.8409   77.0000  -30.0000 42
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0722835000
_diffrn_orient_matrix_UB_12      -0.0934764000
_diffrn_orient_matrix_UB_13      0.0457931000
_diffrn_orient_matrix_UB_21      -0.1631037000
_diffrn_orient_matrix_UB_22      -0.0692716000
_diffrn_orient_matrix_UB_23      -0.0504951000
_diffrn_orient_matrix_UB_31      0.2626732000
_diffrn_orient_matrix_UB_32      -0.0174677000
_diffrn_orient_matrix_UB_33      -0.0441221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3296
_diffrn_reflns_theta_full        61.20
_diffrn_reflns_theta_max         61.20
_diffrn_reflns_theta_min         4.10
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.755
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.6154
_exptl_crystal_description       needle
_exptl_crystal_F_000             602.2935
_exptl_crystal_size_max          0.5977
_exptl_crystal_size_mid          0.0244
_exptl_crystal_size_min          0.0143
_refine_diff_density_max         0.4194
_refine_diff_density_min         -0.3751
_refine_diff_density_rms         0.0559
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_d_res_high            0.8798
_refine_ls_d_res_low             10.7758
_refine_ls_goodness_of_fit_ref   1.0713
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0713
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.7875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.700
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              21
_reflns_limit_l_min              -20
_reflns_number_gt                1486
_reflns_number_total             1625
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5ce01658d2.cif
_cod_data_source_block           6_Li-14hnaq_120K
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7223763
_chemical_oxdiff_formula         'Li C14 O6 N H8'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.2(3) -0.2(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Riding coordinates:
 O6(H6a,H6b)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C12(H12), C11(H11), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'