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_7223549
_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(C196 H168 N16 Ni12 O64)'
_chemical_formula_sum            'C49 H42 N4 Ni3 O16'
_chemical_formula_weight         1118.99
_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             2015-09-07
_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                 113.518(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.505(2)
_cell_length_b                   10.3482(9)
_cell_length_c                   29.521(4)
_cell_measurement_reflns_used    896
_cell_measurement_temperature    293.64(10)
_cell_measurement_theta_max      20.8940
_cell_measurement_theta_min      3.9450
_cell_volume                     5743.7(13)
_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      293.64(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    8.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 33

  2 omega  -42.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -77.0000   30.0000 90

  3 omega   -7.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   77.0000  150.0000 98
;
_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      0.0252333000
_diffrn_orient_matrix_UB_12      -0.0498091000
_diffrn_orient_matrix_UB_13      0.0031802000
_diffrn_orient_matrix_UB_21      0.0274750000
_diffrn_orient_matrix_UB_22      0.0467619000
_diffrn_orient_matrix_UB_23      0.0062477000
_diffrn_orient_matrix_UB_31      0.0056784000
_diffrn_orient_matrix_UB_32      -0.0053146000
_diffrn_orient_matrix_UB_33      0.0252598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_unetI/netI     0.2309
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            12802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74925
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0784P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2601
_reflns_number_total             5648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02254a2.cif
_cod_data_source_block           239-9ni1
_cod_depositor_comments
'Adding full bibliography for 7223544--7223552.cif.'
_cod_database_code               7223549
_reflns_odcompleteness_completeness 99.73
_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, All O(H,H) groups
2. Restrained distances
 H7B-O7
 0.86 with sigma of 0.01
 H7A-O7
 0.86 with sigma of 0.01
 H7B-H7A
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C25A) \\sim Ueq,
Uanis(C21A) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C24B) \\sim Ueq,
Uanis(C21B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5) C24A(0.5) H24A(0.5)
 C25A(0.5) H25A(0.5) C21B(0.5) H21B(0.5) C22B(0.5) H22B(0.5) C23(0.5) H23(0.5)
 H23A(0.5) C23B(0.5) H23B(0.5) C24B(0.5) H24B(0.5)
5.a Riding coordinates:
 O8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21A(H21A), C22A(H22A), C24A(H24A),
 C25A(H25A), C21B(H21B), C22B(H22B), C23(H23), C23(H23A), C23B(H23B), C24B(H24B)
5.c Fitted hexagon refined as free rotating group:
 C21B(C22B,C23,C23B,C24B,N2)
;
_shelx_res_checksum              10541
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-06-04
_olex2_submission_special_instructions 'No special instructions were received'