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_7120816
_publ_section_title
;
 Chiral binary metal-organic frameworks for asymmetric sequential
 reactions
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06979K
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C106 H118 Cd2 Mn2 N12 O18.71 V'
_chemical_formula_sum            'C106 H118 Cd2 Mn2 N12 O18.71 V'
_chemical_formula_weight         2245.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1p8k1k
_audit_creation_date             2016-09-20
_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                   34.7570(10)
_cell_length_b                   17.7053(5)
_cell_length_c                   23.9558(6)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.32
_cell_measurement_theta_min      3.14
_cell_volume                     14742.0(7)
_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      100.01
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53769
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        47.355
_diffrn_reflns_theta_max         47.355
_diffrn_reflns_theta_min         2.240
_exptl_absorpt_coefficient_mu    4.560
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_description       block
_exptl_crystal_F_000             4627
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 4608 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.249(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         13279
_refine_ls_number_restraints     2496
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0811P)^2^+72.4940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                11741
_reflns_number_total             13279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06979k2.cif
_cod_data_source_block           MOF-1
_cod_database_code               7120816
_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
2. Restrained distances
 C102-C103 = C102-C105 = C104-C102
 1.53 with sigma of 0.02
 C92-C90 = C93-C90 = C91-C90
 1.53 with sigma of 0.02
 C102-C98
 1.51 with sigma of 0.02
 C88-C90
 1.51 with sigma of 0.02
 C52-C55 = C52-C54 = C52-C53
 1.53 with sigma of 0.02
 C71-C68 = C70-C68 = C68-C69
 1.53 with sigma of 0.02
 C52-C50
 1.51 with sigma of 0.02
 C64-C68
 1.51 with sigma of 0.02
 C16-C14 = C17-C14 = C15-C14 = C30-C32 = C33-C30 = C30-C31
 1.53 with sigma of 0.02
 C28-C30 = C12-C14
 1.51 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(N7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Mn1A)=1-FVAR(1)
 Sof(O17A)=0.5*(1-FVAR(2))
 Sof(Mn1)=Sof(O17)=FVAR(1)
 Sof(Mn2A)=1-FVAR(2)
 Sof(O18A)=0.5*(1-FVAR(3))
 Sof(Mn2)=Sof(O18)=FVAR(2)
 Sof(O19A)=Sof(V2)=1-FVAR(3)
 Sof(O19)=Sof(V1)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C77(H77), C1(H1), C39(H39), C78(H78), C2(H2), C40(H40)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C41(H41A,H41B), C43(H43A,H43B), C6(H6A,H6B), C79(H79A,H79B),
 C44(H44A,H44B), C42(H42A,H42B), C82(H82A,H82B), C4(H4A,H4B), C3(H3A,H3B),
 C81(H81A,H81B), C80(H80A,H80B)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C22(H22), C21(H21), C101(H101), C99(H99), C85(H85),
 C87(H87), C11(H11), C9(H9), C59(H59), C60(H60), C57(H57), C58(H58), C38(H38),
 C35(H35), C36(H36), C37(H37), C49(H49), C47(H47), C27(H27), C25(H25), C67(H67),
  C65(H65), C61(H61), C76(H76), C73(H73), C74(H74), C75(H75), C23(H23),
 C45(H45), C7(H7), C95(H95), C83(H83)
6.d Fitted hexagon refined as free rotating group:
 C100(C101,C96,C97,C98,C99), C85(C86,C87,C88,C89,C84), C10(C11,C12,C13,C8,C9),
 C59(C60,C56,C57,C58,N8), C38(C34,C35,C36,N4,C37), C26(C27,C28,C29,C24,C25),
 C62(C67,C66,C65,C64,C63)
6.e Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C71(H71A,H71B,
 H71C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C70(H70A,H70B,H70C), C69(H69A,
 H69B,H69C), C55(H55A,H55B,H55C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C104(H10A,H10B,
 H10C), C103(H10D,H10E,H10F), C105(H10G,H10H,H10I), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              74192
_shelx_fab_checksum              92609
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'