Exploring biphenyl-2,4,4′-tricarboxylic acid as a flexible building block for the hydrothermal self-assembly of diverse metal‒organic and supramolecular networks
Shao, Yong-Liang; Cui, Yan-Hui; Gu, Jin-Zhong; Wu, Jiang; Wang, Ya-Wen; Kirillov, Alexander M.; CrystEngComm 18 (2016) 765–; doi:10.1039/C5CE02254A

data_7223550
_publ_section_title
;
 Exploring biphenyl-2,4,4&#x2032;-tricarboxylic acid as a flexible
 building block for the hydrothermal self-assembly of diverse
 metal--organic and supramolecular networks
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              765
_journal_paper_doi               10.1039/C5CE02254A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.25(C200 H168 Co12 N16 O64), 2(C5 H5 N)'
_chemical_formula_sum            'C60 H52 Co3 N6 O16'
_chemical_formula_weight         1289.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-02 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.51(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.600(5)
_cell_length_b                   10.4271(11)
_cell_length_c                   29.646(5)
_cell_measurement_reflns_used    895
_cell_measurement_temperature    297.16(10)
_cell_measurement_theta_max      21.1820
_cell_measurement_theta_min      3.8920
_cell_volume                     5839(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_environment      air
_diffrn_ambient_temperature      297.16(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   30.0000 33

  2 omega  -19.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   19.0000  -90.0000 107

  3 omega  -32.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000   60.0000 78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0291518000
_diffrn_orient_matrix_UB_12      0.0360804000
_diffrn_orient_matrix_UB_13      -0.0000599000
_diffrn_orient_matrix_UB_21      -0.0200984000
_diffrn_orient_matrix_UB_22      0.0181828000
_diffrn_orient_matrix_UB_23      -0.0247472000
_diffrn_orient_matrix_UB_31      -0.0125588000
_diffrn_orient_matrix_UB_32      0.0546788000
_diffrn_orient_matrix_UB_33      0.0082758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_unetI/netI     0.1848
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10401
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.0829
_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^)+(0.0665P)^2^+2.2581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2598
_reflns_number_total             5169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02254a2.cif
_cod_data_source_block           241-8co1
_cod_depositor_comments
'Adding full bibliography for 7223544--7223552.cif.'
_cod_original_cell_volume        5840(2)
_cod_database_code               7223550
_reflns_odcompleteness_completeness 99.72
_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 O(H,H) groups
2. Restrained distances
 H8A-O8
 0.86 with sigma of 0.01
 O8-H8B
 0.86 with sigma of 0.01
 H8A-H8B
 1.48 with sigma of 0.01
3. Rigid bond restraints
 N3, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30 \\sim N3: within 1.2A with sigma of 0.02 and sigma for terminal atoms of
0.04
C16 \\sim N1: within 1.2A with sigma of 0.02 and sigma for terminal atoms of
0.05
C20 \\sim N1: within 1.2A with sigma of 0.02 and sigma for terminal atoms of
0.05
Uanis(C26') \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27') \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29') \\sim Ueq, Uanis(C30') \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H28(0.5) H28A(0.5) C26'(0.5) H26'(0.5) C27'(0.5) H27'(0.5)
 C29'(0.5) H29'(0.5) C30'(0.5) H30'(0.5) C29(0.5) H29(0.5) C26(0.5) H26(0.5)
 C27(0.5) H27(0.5) C30(0.5) H30(0.5)
6.a Rotating group:
 O7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C28(H28A), C26'(H26'), C27'(H27'), C29'(H29'), C30'(H30'),
  C29(H29), C26(H26), C27(H27), C30(H30)
;
_shelx_res_checksum              52960
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'