Highly efficient 3d/4d-4f coordination polymer catalysts for carbon dioxide fixation into cyclic carbonates.
Wang, Gang; Xu, Cong; Wang, Li; Liu, Weisheng; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12711–12717; doi:10.1039/c8dt02576b

data_7047172
_publ_section_title
;
 Highly efficient 3d/4d-4f coordination polymer catalysts for carbon
 dioxide fixation into cyclic carbonates.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12711
_journal_page_last               12717
_journal_paper_doi               10.1039/c8dt02576b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C56 H73 Dy N4 O13 Zn, C57 H76 Dy N4 O13 Zn, 2(C H4 O), C2 H3 N'
_chemical_formula_sum            'C117 H160 Dy2 N9 O28 Zn2'
_chemical_formula_weight         2596.27
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-08 deposited with the CCDC.
2018-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.528(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7435(11)
_cell_length_b                   30.6695(7)
_cell_length_c                   27.5210(15)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.4480
_cell_measurement_theta_min      2.3180
_cell_volume                     14354.6(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5368
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     10.00  35.00   1.00    5.00    --  -40.98  77.00  90.00   25
  2  \w    -67.00  32.00   1.00    5.00    --  -40.98  57.00 -30.00   99
  3  \w    -73.00 -46.00   1.00    5.00    --  -40.98  77.00  90.00   27
  4  \w    -91.00  -3.00   1.00    5.00    --  -40.98 125.00 150.00   88
  5  \w     82.00 135.00   1.00   10.00    --  106.95  45.00  30.00   53
  6  \w     81.00 173.00   1.00   10.00    --  106.95  45.00 -60.00   92
  7  \w     97.00 178.00   1.00   10.00    --  106.95 125.00-180.00   81
  8  \w     33.00 128.00   1.00   10.00    --  106.95 -30.00 120.00   95
  9  \w     75.00 102.00   1.00   10.00    --  106.95 -94.00 -30.00   27
 10  \w     42.00  68.00   1.00   10.00    --  106.95 -94.00 -30.00   26
 11  \w     38.00 105.00   1.00   10.00    --  106.95 -94.00 120.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0132665000
_diffrn_orient_matrix_UB_12      -0.0283654000
_diffrn_orient_matrix_UB_13      0.0485505000
_diffrn_orient_matrix_UB_21      -0.0761783000
_diffrn_orient_matrix_UB_22      -0.0067000000
_diffrn_orient_matrix_UB_23      -0.0326666000
_diffrn_orient_matrix_UB_31      0.0216351000
_diffrn_orient_matrix_UB_32      -0.0408898000
_diffrn_orient_matrix_UB_33      -0.0283189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56836
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.122
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.372
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             5364
_exptl_crystal_recrystallization_method ?????
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.582
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         27803
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1303P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18199
_reflns_number_total             27803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02576b2.cif
_cod_data_source_block           p21nnn
_cod_depositor_comments
'Adding full bibliography for 7047172--7047174.cif.'
_cod_database_code               7047172
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.469
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2. Restrained distances
 C105-C106
 1.25 with sigma of 0.02
 C106-C105
 1.25 with sigma of 0.02
 C107-C108
 1.25 with sigma of 0.02
 C108-C107
 1.25 with sigma of 0.02
 O20-C107
 1.25 with sigma of 0.02
 C107-O20
 1.25 with sigma of 0.02
 C107-O19
 1.25 with sigma of 0.02
 O19-C107
 1.25 with sigma of 0.02
 O27-C114
 1.35 with sigma of 0.02
 C114-O27
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C100) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C101) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C115)
\\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C106)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C107) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(C108)
\\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C69) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O22)
\\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C41(H41A,H41B), C67(H67A,H67B), C93(H93A,H93B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16),
 C29(H29), C31(H31), C33(H33), C38(H38), C40(H40), C42(H42), N6(H6), N8(H8),
 C55(H55), C57(H57), C59(H59), C64(H64), C66(H66), C68(H68), C81(H81), C83(H83),
  C85(H85), C90(H90), C92(H92), C94(H94)
4.c X=CH2 refined with riding coordinates:
 C17(H17A,H17B), C43(H43A,H43B), C69(H69A,H69B), C95(H95A,H95B)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C106(H10P,H10Q,
 H10R), C109(H10S,H10T,H10U), C112(H11J,H11K,H11L), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C97(H97A,H97B,H97C), C98(H98A,
 H98B,H98C), C99(H99A,H99B,H99C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F),
 C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C108(H10M,H10N,H10O), C110(H11A,
 H11B,H11C), C111(H11D,H11E,H11F), C113(H11G,H11H,H11I), C114(H11M,H11N,H11O),
 C117(H11P,H11Q,H11R), C115(H11S,H11T,H11U)
4.e Idealised tetrahedral OH refined as rotating group:
 O27(H27), O28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.645