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_7047174
_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
'C55 H74 Cd Dy N4 O13, C56 H73 Cd1.02 Dy N4 O12, C2 H3 N'
_chemical_formula_sum            'C113 H150 Cd2.02 Dy2 N9 O25'
_chemical_formula_weight         2586.18
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-23 deposited with the CCDC.
2018-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.014(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5629(9)
_cell_length_b                   30.9876(7)
_cell_length_c                   27.6893(14)
_cell_measurement_reflns_used    18980
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.4360
_cell_measurement_theta_min      2.4990
_cell_volume                     14385.8(11)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     18.00  49.00   1.00   17.50    --   11.74 -99.00  90.00   31
  2  \w      7.00  66.00   1.00   17.50    --   11.74  37.00-180.00   59
  3  \w    -21.00  88.00   1.00   17.50    --   11.74  77.00-120.00  109
;
_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      -0.0063383000
_diffrn_orient_matrix_UB_12      -0.0073346000
_diffrn_orient_matrix_UB_13      0.0260830000
_diffrn_orient_matrix_UB_21      -0.0359438000
_diffrn_orient_matrix_UB_22      -0.0027982000
_diffrn_orient_matrix_UB_23      -0.0126630000
_diffrn_orient_matrix_UB_31      0.0068667000
_diffrn_orient_matrix_UB_32      -0.0215068000
_diffrn_orient_matrix_UB_33      -0.0072293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.1037
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            70165
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.928
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84354
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             5279
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.715
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1443
_refine_ls_number_reflns         28253
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+2.0141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16532
_reflns_number_total             28253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02576b2.cif
_cod_data_source_block           wg03
_cod_depositor_comments
'Adding full bibliography for 7047172--7047174.cif.'
_cod_database_code               7047174
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.841
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26A,H26B} of C26, {H52A,H52B} of C52, {H24A,H24B} of C24,
   {H50A,H50B} of C50, {H80A,H80B} of C80, {H10J,H10K} of C106, {H10L,H10M} of
  C108, {H82A,H82B} of C82, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H10U,H10V} of C103, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C56-C55
 1.5 with sigma of 0.02
 C55-O12
 1.2 with sigma of 0.02
 C55-O11
 1.2 with sigma of 0.02
 C24-C25
 1.45 with sigma of 0.02
 O22-H22
 0.87 with sigma of 0.01
 O10-H10
 0.87 with sigma of 0.01
 C25-C26
 1.5 with sigma of 0.02
 C109-H22
 1.993584 with sigma of 0.02
 Dy2-H22
 3.048987 with sigma of 0.02
 C53-H10
 1.918656 with sigma of 0.02
 Dy1-H10
 3.025031 with sigma of 0.02
3. Rigid bond restraints
 C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C76, O21, C111
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C76, C79
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C24 \\sim C25: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C76 \\sim O21 \\sim C111: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
C76 \\sim C79: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C102) \\sim Ueq, Uanis(C7AA) \\sim Ueq, Uanis(C9AA) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(O4) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C106)
\\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C113) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(O21) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C60) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(O21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C7AA(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C9AA(0.5) H9AA(0.5)
 H9AB(0.5) H9AC(0.5) C105(0.5) H10N(0.5) H10O(0.5) H10P(0.5) C104(0.5)
 H10Q(0.5) H10R(0.5) H10S(0.5) C2BA(0.5) H2BA(0.5) H2BB(0.5) H2BC(0.5)
 C103(0.5) H10T(0.5) H10U(0.5) H10V(0.5)
6.a Rotating group:
 O25(H25A,H25B), O21(H21A,H21B)
6.b Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C106(H10J,H10K), C24(H24A,H24B), C50(H50A,H50B)
6.c Aromatic/amide H refined with riding coordinates:
 N8(H8), C89(H89), C85(H85), C87(H87), C70(H70), C63(H63), C94(H94), C96(H96),
 C68(H68), C61(H61), C59(H59), C81(H81), C107(H107), N4(H4), C5(H5), C29(H29),
 C7(H7), C31(H31), C33(H33), C14(H14), C3(H3), C36(H36), C38(H38), C12(H12),
 C51(H51), C25(H25)
6.d X=CH2 refined with riding coordinates:
 C108(H10L,H10M), C82(H82A,H82B), C52(H52A,H52B), C26(H26A,H26B)
6.e Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C74(H74A,H74B,H74C), C100(H10A,H10B,H10C), C73(H73A,H73B,
 H73C), C99(H99A,H99B,H99C), C97(H97A,H97B,H97C), C101(H10D,H10E,H10F),
 C75(H75A,H75B,H75C), C109(H10G,H10H,H10I), C111(H11A,H11B,H11C), C77(H77A,H77B,
 H77C), C7AA(H7AA,H7AB,H7AC), C9AA(H9AA,H9AB,H9AC), C78(H78A,H78B,H78C),
 C44(H44A,H44B,H44C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C), C19(H19A,H19B,
 H19C), C43(H43A,H43B,H43C), C53(H53A,H53B,H53C), C17(H17A,H17B,H17C), C48(H48A,
 H48B,H48C), C54(H54A,H54B,H54C), C21(H21C,H21D,H21E), C47(H47A,H47B,H47C),
 C49(H49A,H49B,H49C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C41(H41A,H41B,
 H41C), C22(H22A,H22B,H22C), C113(H11D,H11E,H11F), C105(H10N,H10O,H10P),
 C104(H10Q,H10R,H10S), C2BA(H2BA,H2BB,H2BC), C103(H10T,H10U,H10V), C56(H56A,
 H56B,H56C), C79(H79A,H79B,H79C)
;
_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 1.237
_oxdiff_exptl_absorpt_empirical_full_min 0.779