Structural diversity of four new metal‒organic frameworks with a curved tetracarboxdiimide dicarboxylic acid
Li, Huimin; Zhou, Jingmin; Shi, Wei; Zhang, Xuejing; Zhang, Zhenjie; Zhang, Meng; Cheng, Peng; CrystEngComm 16 (2014) 834–; doi:10.1039/c3ce41805g

data_7213889
_publ_section_title
;
 Structural diversity of four new metal--organic frameworks with a curved
 tetracarboxdiimide dicarboxylic acid
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              834
_journal_paper_doi               10.1039/c3ce41805g
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C61 H53 Co2 N7 O19'
_chemical_formula_sum            'C61 H53 Co2 N7 O19'
_chemical_formula_weight         1305.96
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                77.071(2)
_cell_angle_beta                 80.672(2)
_cell_angle_gamma                88.411(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4985(3)
_cell_length_b                   21.2760(6)
_cell_length_c                   21.4387(6)
_cell_measurement_reflns_used    16822
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0905
_cell_measurement_theta_min      2.3786
_cell_volume                     5044.0(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -48.00  -18.75   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -77.0000 -120.0000 39

  2 omega  -48.00  -21.00   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -77.0000 -150.0000 36

  3 omega  -12.00   81.00   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000   90.0000 124

  4 omega   10.00   70.00   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000  150.0000 80

  5 omega    3.00   83.25   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000 -120.0000 107

  6 omega  -50.00   43.75   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -77.0000  -30.0000 125
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0344318350
_diffrn_orient_matrix_UB_12      -0.0265811112
_diffrn_orient_matrix_UB_13      0.0195657706
_diffrn_orient_matrix_UB_21      -0.0513252951
_diffrn_orient_matrix_UB_22      0.0142566875
_diffrn_orient_matrix_UB_23      -0.0115758390
_diffrn_orient_matrix_UB_31      0.0100034941
_diffrn_orient_matrix_UB_32      -0.0162219219
_diffrn_orient_matrix_UB_33      -0.0259238420
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33967
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         17764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.139
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                12041
_reflns_number_total             17764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41805g.txt
_cod_data_source_block           1
_cod_database_code               7213889
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C35(H35), C36(H36),
 C37(H37), C40(H40), C41(H41), C42(H42)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C18(H18), C19(H19), C22(H22), C23(H23),
 C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33), C44(H44), C45(H45),
  C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C56(H56), C59(H59)
2.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
;