Chiral porous metal-organic frameworks containing μ-oxo-bis[Ti(salan)] units for asymmetric cyanation of aldehydes.
Du, Xia; Li, Zijian; Liu, Yan; Yang, Shiping; Cui, Yong; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12999–13002; doi:10.1039/c5dt01682g

data_7035520
_publ_section_title
;
 Chiral porous metal-organic frameworks containing \m-oxo-bis[Ti(salan)]
 units for asymmetric cyanation of aldehydes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12999
_journal_page_last               13002
_journal_paper_doi               10.1039/c5dt01682g
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C86 H110 Cd2 N8 O15 Ti2'
_chemical_formula_sum            'C86 H110 Cd2 N8 O15 Ti2'
_chemical_formula_weight         1816.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-08 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9325(12)
_cell_length_b                   26.873(2)
_cell_length_c                   27.147(2)
_cell_measurement_temperature    173(2)
_cell_volume                     10164.1(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_laue_measured_fraction_full 0.822
_diffrn_reflns_laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28745
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.765
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.256
_exptl_absorpt_coefficient_mu    5.059
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 2773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         13756
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.670
_reflns_friedel_fraction_full    0.658
_reflns_friedel_fraction_max     0.675
_reflns_number_gt                9509
_reflns_number_total             13756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01682g2.cif
_cod_data_source_block           mof1_sq
_cod_depositor_comments
'Adding full bibliography for 7035520--7035521.cif.'
_cod_original_cell_volume        10164.2(15)
_cod_database_code               7035520
_audit_block_doi                 10.5517/cc14hyvf
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.751
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C83-C84
 1.51 with sigma of 0.02
3. Rigid bond restraints
 O12, C83
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C83 \\sim C84: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O12 \\sim C83: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
5. Rigid body (RIGU) restrains
 C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N5(H5), N6(H6), C1(H1A), C2(H2A), C39(H39), C40(H40)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C23(H23A,
 H23B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
 C45(H45A,H45B), C61(H61A,H61B)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27), C25(H25),
 C35(H35), C36(H36), C37(H37), C38(H38), C47(H47), C50(H50), C57(H57), C58(H58),
  C59(H59), C60(H60), C65(H65), C63(H63), C76(H76), C75(H75), C74(H74), C73(H73)
6.d Fitted hexagon refined as free rotating group:
 C13(C12,C11,C10,C9,C8), C24(C29,C28,C27,C26,C25), C48(C47,C46,C51,C49,C50),
 C62(C67,C66,C65,C64,C63)
6.e Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C71(H71A,H71B,H71C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C), C80(H80A,H80B,
 H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              65433
_shelx_fab_checksum              91428
_olex2_submission_special_instructions 'No special instructions were received'