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_7226143
_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           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 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                   23.68444(16)
_cell_length_b                   23.68444(16)
_cell_length_c                   46.9716(4)
_cell_measurement_reflns_used    87517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6550
_cell_measurement_theta_min      1.9620
_cell_volume                     26348.8(3)
_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_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (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 0.993
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
  1 omega -109.00   71.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -18.0000  -90.0000 360

  2 omega  -75.50    5.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000  150.0000 161

  3 omega  -64.00   17.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000 -120.0000 162

  4 omega  -56.00   29.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000  -72.0000    0.0000 170

  5 omega   -5.00   15.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000   36.0000  120.0000 40

  6 omega  -67.00  -46.50   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000   72.0000 -180.0000 41

  7 omega  -67.00  -46.50   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000   72.0000  -30.0000 41

  8 omega -109.00   71.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000    0.0000 -120.0000 360

  9 omega  -67.00  -47.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0000   72.0000    0.0000 40
;
_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  0.0748
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            294870
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.861
_diffrn_reflns_theta_min         1.559
_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    0.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56805
_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            pink
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_description       prism
_exptl_crystal_F_000             8336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
To maintain sensible geometry Heavily disordered aliphatic chains were 
geometrically restrained with DFIX/DANG.  
Three heavily disordered --NCS groups have been split and refined over two positions 
each.  One  was refined as isotropic only.
SIMU, SELU and RIGU restraits were used to modell appriopriately 
Atomic Displacement Parameters (ADPs).
Structure is refined as 2-component inversion twin with BASF =0.16(2) 
Highly diffused solvent has been masked out with SMTBX toolbox within OLEX2. 
;
_refine_ls_abs_structure_Flack   0.16(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         26743
_refine_ls_number_restraints     2420
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2652
_refine_ls_wR_factor_ref         0.2836
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                17361
_reflns_number_total             26743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00939e2.cif
_cod_data_source_block           2014ncs0626
_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        26348.8(4)
_cod_database_code               7226143
_chemical_oxdiff_formula         'Co2 C60 H60 N10 O10'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.915
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.84(2) 0.16(2)
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
 C51-C52
 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
 C105-C104
 1.54 with sigma of 0.02
 C104-C103
 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
 C76-C75
 1.54 with sigma of 0.02
 C53-C52
 1.54 with sigma of 0.02
 C112-C111
 0.5 with sigma of 0.01
 N15-C110
 1.2 with sigma of 0.01
 N15-C109
 1.2 with sigma of 0.01
 N15-C109
 1.2 with sigma of 0.01
 N15-C110
 1.2 with sigma of 0.01
 C110-C109
 0.5 with sigma of 0.01
 C109-S4
 1.64 with sigma of 0.01
 C110-S5
 1.64 with sigma of 0.01
 S5-S4
 1.7 with sigma of 0.02
 N16-C114
 1.2 with sigma of 0.01
 N16-C113
 1.2 with sigma of 0.01
 C113-S6
 1.64 with sigma of 0.01
 C114-S7
 1.64 with sigma of 0.01
 C114-C113
 0.5 with sigma of 0.01
 S7-S6
 1.7 with sigma of 0.01
 C103-C102
 1.54 with sigma of 0.01
 C51-C50
 1.54 with sigma of 0.01
 C52-C51
 1.54 with sigma of 0.01
 C52-C53
 1.54 with sigma of 0.01
 C50-C49
 1.54 with sigma of 0.01
 C49-C48
 1.54 with sigma of 0.01
 C102-C103
 1.54 with sigma of 0.01
 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
 C24-C25
 1.54 with sigma of 0.01
 C26-C25
 1.54 with sigma of 0.01
 C24-C23
 1.54 with sigma of 0.01
 C23-C22
 1.54 with sigma of 0.01
 C22-C21
 1.54 with sigma of 0.01
 C107-C105
 2.4 with sigma of 0.04
 C106-C104
 2.4 with sigma of 0.04
 C105-C103
 2.4 with sigma of 0.04
 C104-C102
 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
 C77-C75
 2.4 with sigma of 0.04
 C53-C51
 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(S7) = Uanis(S6)
Uiso(C110) = Uiso(C109) = Uiso(S5) = Uiso(S4)
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(S5)=Sof(C110)=1-FVAR(1)
 Sof(S4)=Sof(C109)=FVAR(1)
 Sof(S7)=Sof(C114)=1-FVAR(2)
 Sof(S6)=Sof(C113)=FVAR(2)
 Sof(C112)=Sof(S2A)=1-FVAR(3)
 Sof(S2)=Sof(C111)=FVAR(3)
8.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C52(H52A,H52B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B),
  C79(H79A,H79B), C102(H10A,H10B), C103(H10C,H10D), C104(H10E,H10F), C105(H10G,
 H10H), C106(H10I,H10J)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C02D(H02D), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C28(H28), C30(H30),
  C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
 C41(H41), C43(H43), C44(H44), C46(H46), C47(H47), C55(H55), C57(H57), C60(H60),
  C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68),
 C70(H70), C71(H71), C73(H73), C74(H74), C82(H82), C84(H84), C87(H87), C88(H88),
  C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95), C97(H97),
 C98(H98), C100(H100), C101(H101)
8.c Fitted hexagon refined as free rotating group:
 C64(C65,C66,N9,C67,C68)
8.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C53(H53A,H53B,H53C), C80(H80A,H80B,H80C), C107(H10K,H10L,
 H10M)
;
_shelx_res_checksum              99043
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'