A Cr(salen)-based metal-organic framework as a versatile catalyst for efficient asymmetric transformations.
Xia, Qingchun; Liu, Yan; Li, Zijian; Gong, Wei; Cui, Yong; Chemical communications (Cambridge, England) 52 (2016) 13167–13170; doi:10.1039/c6cc06019f

data_7124979
_publ_section_title
;
 A Cr(salen)-based metal-organic framework as a versatile catalyst for
 efficient asymmetric transformations.
;
_journal_issue                   89
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13167
_journal_page_last               13170
_journal_paper_doi               10.1039/c6cc06019f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C127 H139 Cd2 Cr4 N8 Na5 O42'
_chemical_formula_sum            'C127 H139 Cd2 Cr4 N8 Na5 O42'
_chemical_formula_weight         2997.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           22
_space_group_name_Hall           'F 2 2'
_space_group_name_H-M_alt        'F 2 2 2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1kmttt
_audit_creation_date             2016-09-12
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-09-14 deposited with the CCDC.
2016-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.623(2)
_cell_length_b                   41.321(2)
_cell_length_c                   51.868(3)
_cell_measurement_reflns_used    9428
_cell_measurement_temperature    116(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.30
_cell_volume                     87065(8)
_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      116.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            116878
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        55.013
_diffrn_reflns_theta_max         55.013
_diffrn_reflns_theta_min         1.747
_exptl_absorpt_coefficient_mu    3.667
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.915
_exptl_crystal_description       block
_exptl_crystal_F_000             24640
_exptl_crystal_preparation       ', '
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.277(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1606
_refine_ls_number_reflns         26170
_refine_ls_number_restraints     2010
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0650
_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^)+(0.1079P)^2^+433.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.2161
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                15111
_reflns_number_total             26170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06019f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        87065(7)
_cod_database_code               7124979
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.723(13) 0.277(13)
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. 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
4. Others
 Fixed Sof: H12D(0.5) H12E(0.5) H12F(0.5) H12G(0.5) H12H(0.5) H12I(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C31(H31), C32(H32), C61(H61), C62(H62), C91(H91), C92(H92)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
  C96(H96A,H96B)
5.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C46(H46A,H46B,H46C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C),
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C106(H10A,H10B,H10C), C107(H10D,H10E,
 H10F), C108(H10G,H10H,H10I), C118(H11A,H11B,H11C), C119(H11D,H11E,H11F),
 C120(H12A,H12B,H12C), C122(H12D,H12E,H12F), C124(H12G,H12H,H12I)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C19(H19), C21(H21), C23(H23), C37(H37), C41(H41),
 C39(H39), C49(H49), C53(H53), C51(H51), C67(H67), C71(H71), C69(H69), C79(H79),
  C83(H83), C85(H85), C97(H97), C99(H99), C101(H101), C109(H109), C113(H113),
 C111(H111)
5.e Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C21(C22,C23,C24,C25,C20), C40(C41,C42,C43,C38,C39),
 C53(C54,C55,C50,C51,C52), C72(C71,C70,C69,C68,C73), C83(C82,C81,C80,C85,C84),
 C98(C99,C100,C101,C102,C103), C115(C114,C113,C112,C111,C110)
5.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C77(H77A,H77B,
 H77C), C88(H88A,H88B,H88C)
;
_shelx_fab_checksum              27570
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'