Chiral binary metal-organic frameworks for asymmetric sequential reactions
Li, Zijian; Liu, Yan; Xia, Qingchun; Cui, Yong; Chem. Commun.  (2017) –; doi:10.1039/C7CC06979K

data_7120815
_publ_section_title
;
 Chiral binary metal-organic frameworks for asymmetric sequential
 reactions
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_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06979K
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C136 H150 Cd2 Fe2 N12 O18.48 V2'
_chemical_formula_sum            'C136 H150 Cd2 Fe2 N12 O18.48 V2'
_chemical_formula_weight         2686.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           17
_space_group_name_Hall           'P 2c 2'
_space_group_name_H-M_alt        'P 2 2 21'
_symmetry_space_group_name_Hall  'P 2c 2'
_symmetry_space_group_name_H-M   'P 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1p8k0j
_audit_creation_date             2016-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-06-20 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1093(6)
_cell_length_b                   34.2098(8)
_cell_length_c                   23.7848(7)
_cell_measurement_reflns_used    2584
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      37.71
_cell_measurement_theta_min      2.57
_cell_volume                     19617.1(9)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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      109.96
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72080
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        50.742
_diffrn_reflns_theta_max         50.742
_diffrn_reflns_theta_min         2.242
_exptl_absorpt_coefficient_mu    3.997
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.910
_exptl_crystal_description       block
_exptl_crystal_F_000             5567
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 5444 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.158(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1456
_refine_ls_number_reflns         20489
_refine_ls_number_restraints     2950
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1508P)^2^+37.8803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2432
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                14960
_reflns_number_total             20489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06979k2.cif
_cod_data_source_block           a_sq
_cod_database_code               7120815
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.740
_olex2_refinement_description
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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
2. Restrained distances
 C90-C92 = C90-C93 = C90-C91 = C102-C105 = C102-C103 = C102-C104
 1.53 with sigma of 0.02
 C70-C68 = C71-C68 = C69-C68
 1.53 with sigma of 0.02
 C30-C26 = C14-C10
 1.51 with sigma of 0.02
 C33-C30 = C32-C30 = C31-C30
 1.53 with sigma of 0.02
 C15-C14 = C16-C14 = C17-C14
 1.53 with sigma of 0.02
 C134-C132 = C133-C132 = C135-C132
 1.53 with sigma of 0.02
 C93-C90 = C92-C90 = C91-C90
 1.53 with sigma of 0.02
 C103-C102 = C104-C102 = C105-C102
 1.53 with sigma of 0.02
 C6-C5
 1.524 with sigma of 0.02
 C5-C4
 1.524 with sigma of 0.02
 N2-C2
 1.45 with sigma of 0.02
 C30-C26
 1.51 with sigma of 0.02
 C110-C109 = C111-C110
 1.524 with sigma of 0.02
 C121-C120 = C123-C120 = C122-C120
 1.53 with sigma of 0.02
 C82-C77
 1.524 with sigma of 0.02
 N10-C78
 1.45 with sigma of 0.02
 C44-C43 = C44-C39
 1.524 with sigma of 0.02
 C42-C41 = C41-C40 = C43-C42
 1.524 with sigma of 0.02
 C98-C102 = C90-C86
 1.51 with sigma of 0.02
 C98-C102 = C90-C86 = C132-C130 = C120-C116
 1.51 with sigma of 0.02
 C96-C95
 1.45 with sigma of 0.02
 C52-C48 = C68-C64
 1.51 with sigma of 0.02
 C56-C50
 1.48 with sigma of 0.02
 H51-H60
 2.1 with sigma of 0.02
 H49-H57
 2.1 with sigma of 0.02
 C55-C52 = C54-C52 = C53-C52
 1.53 with sigma of 0.02
 C55-C53
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(V2A)=Sof(V1A)=Sof(O16A)=Sof(O9A)=1-FVAR(1)
 Sof(O16)=Sof(O9)=0.5*FVAR(2)
 Sof(V2)=Sof(V1)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C108(H108), C2(H2), C40(H40), C107(H107), C1(H1), C39(H39), C78(H78), C77(H77)
6.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C112(H11A,H11B), C43(H43A,H43B), C3(H3A,H3B), C42(H42A,H42B),
 C6(H6A,H6B), C109(H10A,H10B), C111(H11C,H11D), C110(H11E,H11F), C82(H82A,H82B),
  C79(H79A,H79B), C81(H81A,H81B), C80(H80A,H80B), C41(H41A,H41B)
6.c Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C71(H71A,H71B,H71C), C69(H69A,H69B,H69C), C16(H16A,H16B,
 H16C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C105(H10C,H10D,H10E),
 C91(H91A,H91B,H91C), C133(H13G,H13H,H13I), C54(H54A,H54B,H54C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C)
6.d Aromatic/amide H refined with riding coordinates:
 C119(H119), C117(H117), C29(H29), C27(H27), C89(H89), C87(H87), C113(H113),
 C51(H51), C49(H49), C127(H127), C129(H129), C11(H11), C13(H13), C65(H65),
 C67(H67), C125(H125), C59(H59), C58(H58), C57(H57), C60(H60), C45(H45),
 C61(H61), C7(H7), C23(H23), C20(H20), C19(H19), C22(H22), C21(H21), C4(H4),
 C5(H5), C101(H101), C99(H99), C83(H83), C95(H95), C35(H35), C36(H36), C37(H37),
  C38(H38), C76(H76), C75(H75), C74(H74), C73(H73)
6.e Fitted hexagon refined as free rotating group:
 C114(C119,C118,C117,C116,C115), C29(C28,C27,C26,C25,C24), C85(C84,C89,C88,C87,
 C86), C50(C51,C46,C47,C48,C49), C126(C127,C128,C129,C130,C131), C12(C11,C10,C9,
 C8,C13), C62(C63,C64,C65,C66,C67), C59(N7,C58,C57,C56,C60), C20(C19,C18,C22,
 C21,N3), C101(C96,C97,C98,C99,C100), C35(C36,N4,C37,C38,C34), C76(C75,N8,C74,
 C73,C72)
6.f Idealised Me refined as rotating group:
 C122(H12A,H12B,H12C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C134(H13A,
 H13B,H13C), C70(H70A,H70B,H70C), C135(H13D,H13E,H13F), C121(H12D,H12E,H12F),
 C123(H12G,H12H,H12I), C93(H93A,H93B,H93C), C104(H10F,H10G,H10H), C103(H10I,
 H10J,H10K), C92(H92A,H92B,H92C)
;
_shelx_fab_checksum              991
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'