Trace water accelerating the CO2 cycloaddition reaction catalyzed by an indium‒organic framework
Hou, Sheng-Li; Dong, Jie; Jiao, Zhuo-Hao; Jiang, Xiao-Lei; Yang, Xiu-Pei; Zhao, Bin; Inorganic Chemistry Frontiers 5 (2018) 1694–; doi:10.1039/C8QI00260F

data_4349859
_publ_section_title
;
 Trace water accelerating the CO2 cycloaddition reaction catalyzed by an
 indium--organic framework
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1694
_journal_paper_doi               10.1039/C8QI00260F
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         '0.5(C88 H48 In2 N4 O16), H2 O, C2 H8 N'
_chemical_formula_sum            'C46 H34 In N3 O9'
_chemical_formula_weight         887.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-16 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.033(2)
_cell_length_b                   12.713(3)
_cell_length_c                   36.597(7)
_cell_measurement_reflns_used    6654
_cell_measurement_temperature    386(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     5133.2(18)
_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      386.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            47450
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.205
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
TITL 0808 in Pcca #54
CELL   11.0330   12.7130   36.5980     90.00     90.00     90.00
SPGR Pcca
C101 0.750 1.012 0.063 !       2.94 eA-3
C102 0.750 1.002 0.023 !       1.84 eA-3
Q103 0.860 0.026 0.116 !       1.71 eA-3
C104 0.688 0.092 0.062 !       1.57 eA-3
Q105 0.204 0.049 0.086 !       1.32 eA-3
C106 0.849 0.989 0.086 !       1.21 eA-3
Q107 0.782 0.043 0.104 !       1.00 eA-3
C108 0.372 0.987 0.257 !       0.87 eA-3
Q109 0.872 0.099 0.197 !       0.85 eA-3
C110 0.672 0.926 0.230 !       0.84 eA-3
C111 0.276 0.888 0.422 !       0.83 eA-3
Q112 0.797 0.944 0.251 !       0.83 eA-3
C113 0.218 0.052 0.493 !       0.81 eA-3
C114 0.719 0.992 0.241 !       0.78 eA-3
Q115 0.688 0.026 0.400 !       0.76 eA-3
Q116 0.014 0.273 0.303 !       0.75 eA-3
Q117 0.297 0.982 0.116 !       0.71 eA-3
Q118 0.188 0.181 0.229 !       0.69 eA-3
C119 0.640 0.116 0.084 !       0.65 eA-3
Q120 0.077 0.240 0.308 !       0.64 eA-3
Q121 0.907 0.268 0.157 !       0.63 eA-3
Q122 0.408 0.813 0.196 !       0.63 eA-3
Q123 0.516 0.689 0.219 !       0.63 eA-3
Q124 0.221 0.964 0.228 !       0.61 eA-3
Q125 0.682 0.099 0.008 !       0.60 eA-3
Q126 0.518 0.773 0.313 !       0.59 eA-3
Q127 0.797 0.095 0.277 !       0.59 eA-3
Q128 0.876 0.885 0.351 !       0.57 eA-3
Q129 0.206 0.146 0.196 !       0.56 eA-3
Q130 0.283 0.951 0.299 !       0.55 eA-3
Q131 0.185 0.195 0.446 !       0.54 eA-3
Q132 0.690 0.962 0.296 !       0.53 eA-3
Q133 0.472 0.299 0.265 !       0.52 eA-3
Q134 0.718 0.857 0.007 !       0.52 eA-3
Q135 0.621 0.964 0.274 !       0.51 eA-3
Q136 0.922 0.309 0.149 !       0.50 eA-3
;
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5862
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1020P)^2^+15.8444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2413
_refine_ls_wR_factor_ref         0.2604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4124
_reflns_number_total             5862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00260f2.cif
_cod_data_source_block           0808_sq
_cod_original_cell_volume        5133.3(19)
_cod_database_code               4349859
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1B
 0.85 with sigma of 0.02
 C6AA-H1B
 1.7 with sigma of 0.02
 H1A-H1B
 1.6 with sigma of 0.02
 N1-C4
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim N1 \\sim C6AA: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C4, N1, C6AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: O8AA(0.5) H8AA(0.5) H8AB(0.5) N1(0.5) H1A(0.5) H1B(0.5) C6AA(0.5)
 H6AA(0.5) H6AB(0.5) H6AC(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
6.a Riding coordinates:
 O8AA(H8AA,H8AB), N1(H1A,H1B), C4(H4A,H4B,H4C)
6.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C14(H14), C22(H22), C23(H23), C29(H29), C11(H11), C12(H12),
 C13(H13), C15(H15), C8(H8), C5(H5), C3(H3)
6.c Idealised Me refined as rotating group:
 C6AA(H6AA,H6AB,H6AC)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'