Structural diversity of alkali metal coordination polymers driven by flexible biphenyl-4,4′-dioxydiacetic acid
Łyszczek, Renata; Głuchowska, Halina; Mazur, Liliana; Tarasiuk, Bogdan; Kinzhybalo, Vasyl; Kirillov, Alexander M.; Journal of Solid State Chemistry 265 (2018) 92–99; doi:10.1016/j.jssc.2018.05.022

data_1560998
_publ_section_title
;
 Structural diversity of alkali metal coordination polymers driven by
 flexible biphenyl-4,4&#x2032;-dioxydiacetic acid
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              92
_journal_page_last               99
_journal_paper_doi               10.1016/j.jssc.2018.05.022
_journal_volume                  265
_journal_year                    2018
_chemical_formula_moiety         '0.5(C32 H40 Li4 O20)'
_chemical_formula_sum            'C16 H20 Li2 O10'
_chemical_formula_weight         386.20
_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'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 94.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.997(4)
_cell_length_b                   7.901(2)
_cell_length_c                   6.549(2)
_cell_measurement_reflns_used    5223
_cell_measurement_temperature    120
_cell_measurement_theta_max      36.3067
_cell_measurement_theta_min      2.8391
_cell_volume                     876.2(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.581
_diffrn_measurement_details
;
  1 omega  -64.00   71.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000    0.0000 181

  2 omega  -64.00   71.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000   90.0000 181

  3 omega  -64.00   71.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000  180.0000 181

  4 omega  -64.00   71.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  -79.0000  270.0000 181

  5 omega  -46.00    2.75   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000  -79.0000   45.0000 65
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1063200000
_diffrn_orient_matrix_UB_12      -0.0149157000
_diffrn_orient_matrix_UB_13      -0.0014629000
_diffrn_orient_matrix_UB_21      0.0116381000
_diffrn_orient_matrix_UB_22      -0.0084348000
_diffrn_orient_matrix_UB_23      0.0416999000
_diffrn_orient_matrix_UB_31      -0.0194649000
_diffrn_orient_matrix_UB_32      -0.0881208000
_diffrn_orient_matrix_UB_33      -0.0037588000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.581
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7500
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.581
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         36.392
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0491
_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^)+(0.1045P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2059
_reflns_number_total             2479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-265-92.cif
_cod_data_source_block           1
_cod_database_code               1560998
_chemical_oxdiff_formula         C16H20Li2O10
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.940
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All Li(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C4(H4), C7(H7)
;
_shelx_res_checksum              65119
_shelx_hkl_checksum              9995
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'