Heteroleptic, polynuclear dysprosium(iii)-carbamato complexes through in situ carbon dioxide capture.
Schlittenhardt, Sören; Moreno-Pineda, Eufemio; Ruben, Mario; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4735–4742; doi:10.1039/d1dt00063b

data_7706863
_publ_section_title
;
 Heteroleptic, polynuclear dysprosium(iii)-carbamato complexes through in
 situ carbon dioxide capture.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4735
_journal_page_last               4742
_journal_paper_doi               10.1039/d1dt00063b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C100 H166 Dy6 N12 O34, 3(C7 H8), 1[C7 H8]'
_chemical_formula_sum            'C128 H198 Dy6 N12 O34'
_chemical_formula_weight         3423.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-10 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4511(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6199(2)
_cell_length_b                   28.7305(3)
_cell_length_c                   20.34422(16)
_cell_measurement_reflns_used    40906
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      27.1580
_cell_measurement_theta_min      2.0690
_cell_volume                     16129.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_detector                 'imaging plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -90.00  90.00   1.00  240.60    --    0.00 180.00 250.00  180
  2  \w    -70.00 -10.00   1.00  240.60    --    0.00 180.00  34.00   60
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0017426000
_diffrn_orient_matrix_UB_12      0.0246144000
_diffrn_orient_matrix_UB_13      -0.0011016000
_diffrn_orient_matrix_UB_21      0.0222765000
_diffrn_orient_matrix_UB_22      0.0011071000
_diffrn_orient_matrix_UB_23      -0.0160460000
_diffrn_orient_matrix_UB_31      -0.0127082000
_diffrn_orient_matrix_UB_32      -0.0014452000
_diffrn_orient_matrix_UB_33      -0.0309773000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78689
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.736
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             6872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         16463
_refine_ls_number_restraints     404
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+43.9878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14215
_reflns_number_total             16463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00063b2.cif
_cod_data_source_block           sor-10_1
_cod_depositor_comments
'Adding full bibliography for 7706862--7706864.cif.'
_cod_database_code               7706863
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Dy6 N12 O34 C100 H166'
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.540
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C105-C107 \\sim C107-C101
 with sigma of 0.02
 C119-C121 \\sim C121-C115
 with sigma of 0.02
 C112-C111 \\sim C119-C118
 with sigma of 0.02
 C112-C114 \\sim C114-C108
 with sigma of 0.02
 C114-C113 \\sim C121-C120
 with sigma of 0.02
 C112-C113 \\sim C119-C120
 with sigma of 0.02
 C114-C112 \\sim C121-C119
 with sigma of 0.04
 C114-C108 \\sim C121-C115
 with sigma of 0.04
 C31A-N4A \\sim C28A-C31B \\sim N4B-C28B
 with sigma of 0.02
 C111-C110 \\sim C118-C117
 with sigma of 0.02
 C110-C109 \\sim C117-C116
 with sigma of 0.02
 N4A-C27 \\sim C27-N4B
 with sigma of 0.02
 C109-C108 \\sim C116-C115
 with sigma of 0.02
 C29B-C28B \\sim C30B-C29A \\sim C28A-C30A \\sim C32B-C31B \\sim C33B-C32A
\\sim C31A-C33A
 with sigma of 0.02
 C108-C113 \\sim C115-C120
 with sigma of 0.02
 C112-C110 \\sim C119-C117
 with sigma of 0.04
 C112-C108 \\sim C119-C115
 with sigma of 0.04
 C111-C109 \\sim C118-C116
 with sigma of 0.04
 C111-C113 \\sim C118-C120
 with sigma of 0.04
 C110-C108 \\sim C117-C115
 with sigma of 0.04
 C109-C113 \\sim C116-C120
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C121) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C116) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C117) \\sim Ueq,
Uanis(C118) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C110) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C32A) = Uanis(C32B)
Uanis(N4B) = Uanis(N4A)
Uanis(C28B) = Uanis(C28A) = Uanis(C31B) = Uanis(C31A)
Uanis(C28A) = Uanis(C28B)
Uanis(C15) = Uanis(C18)
4. Rigid body (RIGU) restrains
 N4A, C28A, C30A, C29A, C31A, C32A, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C115, C120, C119, C118, C117, C116, C121
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C114, C112, C111, C110, C109, C108, C113
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C36, C37, C38, C39, C40, O15, O14, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4B, C28B, C30B, C29B, C31B, C33B, C32B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C15, C17, N2, C20, C18, C19, C3, O7, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C115)=Sof(H115)=Sof(C120)=Sof(C119)=Sof(H119)=Sof(C118)=Sof(H118)=
 Sof(C117)=Sof(H117)=Sof(C116)=Sof(H116)=Sof(C121)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=0.5*(1-FVAR(2))
 Sof(C114)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C112)=Sof(H112)=Sof(C111)=
 Sof(H111)=Sof(C110)=Sof(H110)=Sof(C109)=Sof(H109)=Sof(C108)=Sof(H108)=
 Sof(C113)=0.5*FVAR(2)
 Sof(N4B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(N4A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
 Sof(C31B)=Sof(H31B)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C32B)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(3)
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C9(H9), C21(H21), C24(H24), C18(H18), C15(H15), C28A(H28A),
 C31A(H31A), C28B(H28B), C31B(H31B)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
6.c Me refined with riding coordinates:
 C32A(H32A,H32B,H32C), C29A(H29A,H29B,H29C), C33A(H33A,H33B,H33C), C30A(H30A,
 H30B,H30C), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C33B(H33D,H33E,H33F),
 C32B(H32D,H32E,H32F)
6.d Aromatic/amide H refined with riding coordinates:
 C48(H48), C47(H47), C46(H46), C39(H39), C38(H38), C37(H37), C50(H50),
 C41A(H41A), C105(H105), C104(H104), C103(H103), C102(H102), C101(H101),
 C112(H112), C111(H111), C110(H110), C109(H109), C108(H108), C115(H115),
 C119(H119), C118(H118), C117(H117), C116(H116)
6.e Fitted hexagon refined as free rotating group:
 C105(C104,C103,C102,C101,C106), C112(C111,C110,C109,C108,C113), C115(C120,
 C119,C118,C117,C116)
6.f Idealised Me refined with riding coordinates:
 C114(H11D,H11E,H11F), C121(H12A,H12B,H12C)
6.g Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C34(H34A,H34B,H34C), C51(H51A,H51B,
 H51C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C11(H11A,
 H11B,H11C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
 C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C107(H10D,H10E,H10F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 208 electrons were 
found in a volume of 1982\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C7H8] per Unit Cell 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68031
_shelx_hkl_checksum              90125
_shelx_fab_checksum              84776
_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 1.177
_oxdiff_exptl_absorpt_empirical_full_min 0.876