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_7226144
_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         'C124 H132 Co2 N16 O4 S4, 2(C H Cl3), C H4 O'
_chemical_formula_sum            'C127 H138 Cl6 Co2 N16 O5 S4'
_chemical_formula_weight         2427.33
_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                   23.88216(9)
_cell_length_b                   23.88216(9)
_cell_length_c                   46.8514(3)
_cell_measurement_reflns_used    151902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5260
_cell_measurement_theta_min      1.9730
_cell_volume                     26722.1(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -112.00   68.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000  -18.0000   90.0000 360

  2 omega  -82.00   22.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000  -72.0000  -30.0000 208

  3 omega -112.00   22.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000  -72.0000  120.0000 268

  4 omega  -55.50  -19.50   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000  -72.0000 -120.0000 72

  5 omega  -66.00  -45.50   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000   72.0000    0.0000 41

  6 omega  -66.00  -45.50   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000   72.0000  150.0000 41

  7 omega  -66.00  -45.50   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000   72.0000  -30.0000 41

  8 omega  -61.00  -38.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000   72.0000  120.0000 46

  9 omega  -66.00  -45.50   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0000   72.0000 -150.0000 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  0.0437
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            292603
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.486
_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    0.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61175
_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    1.207
_exptl_crystal_description       prism
_exptl_crystal_F_000             10176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.841
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Flack x determined using 11610 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.049(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1426
_refine_ls_number_reflns         30625
_refine_ls_number_restraints     2605
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0913
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1815P)^2^+34.5021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2560
_refine_ls_wR_factor_ref         0.2615
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                28191
_reflns_number_total             30625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00939e2.cif
_cod_data_source_block           2014ncs0627
_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        26722.0(3)
_cod_database_code               7226144
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.868
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C52-C53
 1.54 with sigma of 0.02
 C53-C54
 1.54 with sigma of 0.02
 C54-C55
 1.54 with sigma of 0.02
 C55-C56
 1.54 with sigma of 0.02
 C56-C57
 1.54 with sigma of 0.02
 C57-C58
 1.54 with sigma of 0.02
 C58-C59
 1.54 with sigma of 0.02
 C59-C60
 1.54 with sigma of 0.02
 C112-C113
 1.54 with sigma of 0.02
 C113-C114
 1.54 with sigma of 0.02
 C114-C115
 1.54 with sigma of 0.02
 C115-C116
 1.54 with sigma of 0.02
 C116-C117
 1.54 with sigma of 0.02
 C117-C118
 1.54 with sigma of 0.02
 C118-C119
 1.54 with sigma of 0.02
 C120-C119
 1.54 with sigma of 0.02
 C114-C113
 1.54 with sigma of 0.01
 C114-C115
 1.54 with sigma of 0.01
 C27-C28
 1.54 with sigma of 0.01
 C28-C29
 1.54 with sigma of 0.01
 C29-C30
 1.54 with sigma of 0.01
 C118-C120
 2.4 with sigma of 0.02
 C117-C119
 2.4 with sigma of 0.02
 C115-C117
 2.4 with sigma of 0.02
 C114-C116
 2.4 with sigma of 0.02
3. 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
4. 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
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. 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
6. Same fragment restrains
{O1, C22, C23, C24, C25, C26, C27, C28, C29, C30} sigma for 1-2: 0.02, 1-3: 0.04
as
{O4, C112, C113, C114, C115, C116, C117, C118, C119, C121}
{C200, Cl1, Cl2, Cl3} sigma for 1-2: 0.02, 1-3: 0.04
as
{C201, Cl5, Cl6, Cl4}
7.a Ternary CH refined with riding coordinates:
 C200(H200), C201(H201)
7.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
  C58(H58A,H58B), C59(H59A,H59B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,
 H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
 C89(H89A,H89B), C112(H11A,H11B), C113(H11C,H11D), C114(H11E,H11F), C115(H11G,
 H11H), C116(H11I,H11J), C117(H11K,H11L), C118(H11M,H11N), C119(H11O,H11P)
7.c Me refined with riding coordinates:
 C60(H60A,H60B,H60C), C120(H12A,H12B,H12C)
7.d 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), C32(H32), C34(H34),
  C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C62(H62), C64(H64), C67(H67),
  C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75),
 C77(H77), C78(H78), C80(H80), C81(H81), C92(H92), C94(H94), C97(H97), C98(H98),
  C99(H99), C100(H100), C102(H102), C103(H103), C104(H104), C105(H105),
 C107(H107), C108(H108), C110(H110), C111(H111)
7.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C90(H90A,H90B,H90C), C260(H26C,H26D,H26E)
7.f Idealised tetrahedral OH refined as rotating group:
 O52(H52)
;
_shelx_res_checksum              52462
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'