Constructing chiral MOFs by functionalizing 4,2′:6′,4′′-terpyridine with long-chain alkoxy domains: rare examples of neb nets
Klein, Y. Maximilian; Prescimone, Alessandro; Pitak, Mateusz B.; J.Coles, Simon; Constable, Edwin C.; Housecroft, Catherine E.; CrystEngComm 18 (2016) 4704–; doi:10.1039/C6CE00939E

data_7226142
_publ_section_title
;
 Constructing chiral MOFs by functionalizing
 4,2&#x2032;:6&#x2032;,4&#x2032;&#x2032;-terpyridine with long-chain
 alkoxy domains: rare examples of neb nets
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              4704
_journal_paper_doi               10.1039/C6CE00939E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C112 H108 Co2 N16 O4 S4'
_chemical_formula_sum            'C112 H108 Co2 N16 O4 S4'
_chemical_formula_weight         1988.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-15 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.7111(4)
_cell_length_b                   23.7111(4)
_cell_length_c                   46.9783(7)
_cell_measurement_reflns_used    23217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6710
_cell_measurement_theta_min      2.0330
_cell_volume                     26412.0(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
  1 omega  -61.00   70.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   72.0000 -150.0000 262

  2 omega -106.00  -86.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -36.0000 -180.0000 40

  3 omega  -67.50  -47.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -72.0000  -90.0000 41
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            79766
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.221
_diffrn_reflns_theta_min         1.718
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       block
_exptl_crystal_F_000             8336
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.21(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1226
_refine_ls_number_reflns         26290
_refine_ls_number_restraints     2415
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1658P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2552
_refine_ls_wR_factor_ref         0.2795
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                12814
_reflns_number_total             26290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00939e2.cif
_cod_data_source_block           2014ncs0624
_cod_depositor_comments
;
The following automatic conversions were performed:
'__diffrn_detector' tag replaced with '_diffrn_detector' tag.

Automatic conversion script
Id: cif_correct_tags 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        26412.0(9)
_cod_database_code               7226142
_chemical_oxdiff_formula         'Co2 C50 H50 S2 N6 O5'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.961
_reflns_odcompleteness_completeness 96.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.79(3) 0.21(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C107-C108
 1.54 with sigma of 0.02
 C106-C107
 1.54 with sigma of 0.02
 C105-C106
 1.54 with sigma of 0.02
 C104-C105
 1.54 with sigma of 0.02
 C103-C104
 1.54 with sigma of 0.02
 C81-C80
 1.54 with sigma of 0.02
 C80-C79
 1.54 with sigma of 0.02
 C79-C78
 1.54 with sigma of 0.02
 C78-C77
 1.54 with sigma of 0.02
 C77-C76
 1.54 with sigma of 0.02
 C103-C104
 1.54 with sigma of 0.01
 C104-C105
 1.54 with sigma of 0.01
 C105-C106
 1.54 with sigma of 0.01
 C106-C107
 1.54 with sigma of 0.01
 C107-C108
 1.54 with sigma of 0.01
 C81-C80
 1.54 with sigma of 0.01
 C80-C79
 1.54 with sigma of 0.01
 C79-C78
 1.54 with sigma of 0.01
 C78-C77
 1.54 with sigma of 0.01
 C77-C76
 1.54 with sigma of 0.01
 C22-C23
 1.54 with sigma of 0.01
 C23-C24
 1.54 with sigma of 0.01
 C24-C25
 1.54 with sigma of 0.01
 C25-C26
 1.54 with sigma of 0.01
 C26-C27
 1.54 with sigma of 0.01
 N16-C113
 1.2 with sigma of 0.01
 N16A-C114
 1.2 with sigma of 0.01
 C113-S4
 1.64 with sigma of 0.01
 C114-S4A
 1.64 with sigma of 0.01
 Co3-N16
 2.1 with sigma of 0.01
 Co3-N16A
 2.1 with sigma of 0.01
 S4A-S4
 1.7 with sigma of 0.02
 C114-C113
 0.7 with sigma of 0.02
 Co2-N15
 2.1 with sigma of 0.01
 Co2-N15A
 2.1 with sigma of 0.01
 C112-N15
 1.2 with sigma of 0.01
 N15A-C111
 1.2 with sigma of 0.01
 C111-S3A
 1.64 with sigma of 0.01
 C112-S3
 1.64 with sigma of 0.01
 C97-C84
 1.46 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.01
 C53-C54
 1.54 with sigma of 0.01
 C52-C51
 1.54 with sigma of 0.01
 C51-C50
 1.54 with sigma of 0.01
 C50-C49
 1.54 with sigma of 0.01
 C1-C6
 1.46 with sigma of 0.01
 C106-C108
 2.4 with sigma of 0.04
 C81-C79
 2.4 with sigma of 0.04
 C80-C78
 2.4 with sigma of 0.04
 C79-C77
 2.4 with sigma of 0.04
 C78-C76
 2.4 with sigma of 0.04
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C114) = Uanis(C113)
Uanis(S4A) = Uanis(S4)
Uanis(N16) = Uanis(N16A)
Uanis(N15A) = Uanis(N15)
Uanis(C111) = Uanis(C112)
Uanis(S3) = Uanis(S3A)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(N16A)=Sof(C114)=Sof(S4A)=1-FVAR(1)
 Sof(N16)=Sof(C113)=Sof(S4)=FVAR(1)
 Sof(N15A)=Sof(S3A)=1-FVAR(2)
 Sof(S3)=Sof(N15)=FVAR(2)
 Sof(C112)=1-FVAR(3)
 Sof(C111)=FVAR(3)
8.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
  C80(H80A,H80B), C103(H10A,H10B), C104(H10C,H10D), C105(H10E,H10F), C106(H10G,
 H10H), C107(H10I,H10J)
8.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C54(H54A,H54B,H54C), C81(H81A,H81B,H81C), C108(H10K,H10L,
 H10M)
8.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C29(H29), C31(H31),
  C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
 C42(H42), C44(H44), C45(H45), C47(H47), C48(H48), C56(H56), C58(H58), C61(H61),
  C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69),
 C71(H71), C72(H72), C74(H74), C75(H75), C83(H83), C85(H85), C88(H88), C89(H89),
  C90(H90), C91(H91), C93(H93), C94(H94), C95(H95), C96(H96), C98(H98),
 C99(H99), C101(H101), C102(H102)
;
_shelx_res_checksum              8063
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'