A Mesoporous Indium Metal-Organic Framework: Remarkable Advances in Catalytic Activity for Strecker Reaction of Ketones.
Reinares-Fisac, Daniel; Aguirre-Díaz, Lina María; Iglesias, Marta; Snejko, Natalia; Gutiérrez-Puebla, Enrique; Monge, M Ángeles; Gándara, Felipe; Journal of the American Chemical Society 138 (2016) 9089–9092; doi:10.1021/jacs.6b05706

data_4130656
_publ_section_title
;
 A Mesoporous Indium Metal-Organic Framework: Remarkable Advances in
 Catalytic Activity for Strecker Reaction of Ketones.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9089
_journal_page_last               9092
_journal_paper_doi               10.1021/jacs.6b05706
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '0.5(C348 H195 In18 N3 O93), 3.82(C3.67)'
_chemical_formula_sum            'C188 H97.5 In9 N1.5 O46.5'
_chemical_formula_weight         4154.55
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   31.7180(15)
_cell_length_b                   31.7180(15)
_cell_length_c                   17.1352(9)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    250.0
_cell_measurement_theta_max      62.527
_cell_measurement_theta_min      2.786
_cell_volume                     14929.0(13)
_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      250.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1249
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            119004
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.200
_diffrn_reflns_theta_max         65.200
_diffrn_reflns_theta_min         1.608
_exptl_absorpt_coefficient_mu    5.846
_exptl_absorpt_correction_T_max  0.5835
_exptl_absorpt_correction_T_min  0.3529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1547 before and 0.0950 after correction.
The Ratio of minimum to maximum transmission is 0.6048.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.924
_exptl_crystal_description       prism
_exptl_crystal_F_000             4098
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.744
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.221
_refine_ls_abs_structure_details
;
 Flack x determined using 2978 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.114(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8819
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+9.5111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1939
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7519
_reflns_number_total             8819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05706_si_003.cif
_cod_data_source_block           version1p_62c_a
_cod_original_cell_volume        14929.0(16)
_cod_original_formula_sum        'C188 H97.50 In9 N1.50 O46.50'
_cod_database_code               4130656
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6) = Uanis(N1)
3. Others
 Fixed Sof: N1(0.25) C1AA(0.25) C2(0.25) H2(0.25) C3(0.25) H3(0.25) C5(0.25)
 H5(0.25) C16(0.25) H16(0.25) C29(0.25) H29(0.25) C9(0.33333) C11(0.25)
 C14(0.33333) C15(0.33333) C17(0.16667) C19(0.33333) C33(0.33333) O6(0.25)
 C0AA(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C014(H014), C016(H016), C2(H2), C3(H3), C5(H5), C16(H16), C29(H29), C1(H1),
 C24(H24)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'