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_7706864
_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
'C163.947 H165.947 Dy6 N12 O34, 1(C7 H8), 1.5[C7H8]'
_chemical_formula_sum            'C181.45 H185.95 Dy6 N12 O34'
_chemical_formula_weight         4053.76
_chemical_properties_physical    Moisture-sensitive
_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'
_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                 97.1774(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.05782(16)
_cell_length_b                   20.9377(2)
_cell_length_c                   29.0794(3)
_cell_measurement_reflns_used    40096
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      27.0580
_cell_measurement_theta_min      1.8210
_cell_volume                     9096.20(16)
_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   0.80  240.60    --    0.00 180.00 242.00  225
;
_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      -0.0061502000
_diffrn_orient_matrix_UB_12      0.0259929000
_diffrn_orient_matrix_UB_13      -0.0157139000
_diffrn_orient_matrix_UB_21      0.0124358000
_diffrn_orient_matrix_UB_22      0.0215825000
_diffrn_orient_matrix_UB_23      0.0184865000
_diffrn_orient_matrix_UB_31      0.0454065000
_diffrn_orient_matrix_UB_32      -0.0023774000
_diffrn_orient_matrix_UB_33      -0.0039885000
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            64483
_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         26.372
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89084
_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    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             4053
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.151
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         18589
_refine_ls_number_restraints     551
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0701P)^2^+7.6460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15781
_reflns_number_total             18589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00063b2.cif
_cod_data_source_block           sor-28d
_cod_depositor_comments
'Adding full bibliography for 7706862--7706864.cif.'
_cod_original_cell_volume        9096.21(16)
_cod_database_code               7706864
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Dy6 N12 O34 C164 H166'
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.534
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C310-C308 \\sim C308-C314
 with sigma of 0.02
 C47A-C46A \\sim C46C-C28 \\sim C46B-C47B
 with sigma of 0.02
 C46A-N4 \\sim C46B-N4 \\sim C46C-N4
 with sigma of 0.02
 C39A-N4 \\sim N4-C39B
 with sigma of 0.02
 C39B-C40B \\sim C39A-C40A
 with sigma of 0.02
 C303-C301 \\sim C301-C307
 with sigma of 0.02
 C24A-N3 \\sim N3-C24B
 with sigma of 0.02
 C31B-N3 \\sim N3-C31A
 with sigma of 0.02
 C77B-C76 \\sim C76-C77A
 with sigma of 0.02
3. Restrained planarity
 C304, C302, C307, C301, C303, C305, C306
 with sigma of 0.1
 C312, C308, C311, C313, C314, C309, C310
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C304) \\sim Ueq, Uanis(C302) \\sim Ueq, Uanis(C307) \\sim Ueq,
Uanis(C301) \\sim Ueq, Uanis(C303) \\sim Ueq, Uanis(C305) \\sim Ueq,
Uanis(C306) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C308) \\sim Ueq, Uanis(C309) \\sim Ueq, Uanis(C314) \\sim Ueq,
Uanis(C310) \\sim Ueq, Uanis(C313) \\sim Ueq, Uanis(C311) \\sim Ueq,
Uanis(C312) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C50A) = Uanis(C48C) = Uanis(C50B)
Uanis(C49A) = Uanis(C25) = Uanis(C49B)
Uanis(C51A) = Uanis(C27) = Uanis(C51B)
Uanis(C48B) = Uanis(C24) = Uanis(C48A)
Uanis(C52A) = Uanis(C26) = Uanis(C52B)
Uanis(C47A) = Uanis(C28) = Uanis(C47B)
Uanis(C46A) = Uanis(C46C) = Uanis(C46B)
Uanis(C31A) = Uanis(C31B)
5. Rigid body (RIGU) restrains
 C47B, C52B, C51B, C50B, C49B, C48B, C46B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C47A, C48A, C49A, C50A, C51A, C52A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C39B, C40B, C41B, C42B, C43B, C44B, C45B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3, C24B, C25B, C26B, C27B, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32B, C33B, C34B, C35B, C36B, C37B, C31B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55, C56, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C25A, C26A, C27A, C28A, C29A, C30A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32A, C33A, C34A, C35A, C36A, C37A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C77A, C82A, C81A, C80A, C79A, C78A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C40A, C45A, C44A, C43A, C42A, C41A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C77B, C82B, C81B, C80B, C79B, C78B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 1*[Sof(C301)+Sof(H30C)+Sof(H30D)+Sof(H30E)+Sof(C306)+Sof(H306)+Sof(C307)+
 Sof(H307)+Sof(C302)+Sof(C303)+Sof(H303)+Sof(C304)+Sof(H304)+Sof(C305)+
 Sof(H305)]+1*[Sof(C308)+Sof(H30F)+Sof(H30G)+Sof(H30H)+Sof(C311)+Sof(H311)+
 Sof(C312)+Sof(H312)+Sof(C313)+Sof(H313)+Sof(C314)+Sof(H314)+Sof(C309)+
 Sof(C310)+Sof(H310)]=0.5 with esd of 0.00001
 1*[Sof(C46A)+Sof(H46A)+Sof(H46B)+Sof(C52A)+Sof(H52A)+Sof(C51A)+Sof(H51A)+
 Sof(C50A)+Sof(H50A)+Sof(C49A)+Sof(H49A)+Sof(C48A)+Sof(H48A)+Sof(C47A)]+1*
 [Sof(C46B)+Sof(H46C)+Sof(H46D)+Sof(C47B)+Sof(C52B)+Sof(H52B)+Sof(C51B)+
 Sof(H51B)+Sof(C50B)+Sof(H50B)+Sof(C49B)+Sof(H49B)]+1*[Sof(C27)+Sof(H27)+
 Sof(C26)+Sof(H26)+Sof(C28)+Sof(C24)+Sof(H24)+Sof(C25)+Sof(H25)+Sof(C48C)+
 Sof(H48C)+Sof(C46C)+Sof(H46E)+Sof(H46F)]=1 with esd of 0.00001
 Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(C37B)=Sof(H37B)=Sof(C36B)=
 Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C34B)=Sof(H34B)=Sof(C33B)=Sof(H33B)=1-FVAR(1)
 Sof(C32A)=Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=
 Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=FVAR(1)
 Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(C52A)=Sof(H52A)=Sof(C51A)=Sof(H51A)=
 Sof(C50A)=Sof(H50A)=Sof(C49A)=Sof(H49A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=FVAR(2)
 Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(C45B)=Sof(H45B)=Sof(C44B)=
 Sof(H44B)=Sof(C43B)=Sof(H43B)=Sof(C42B)=Sof(H42B)=Sof(C41B)=Sof(H41B)=1-FVAR(3)
 Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(C45A)=Sof(H45A)=Sof(C44A)=
 Sof(H44A)=Sof(C43A)=Sof(H43A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=FVAR(3)
 Sof(H76C)=Sof(H76D)=Sof(C77B)=Sof(C82B)=Sof(H82B)=Sof(C81B)=Sof(H81B)=
 Sof(C80B)=Sof(H80B)=Sof(C79B)=Sof(H79B)=Sof(C78B)=Sof(H78B)=1-FVAR(4)
 Sof(H76A)=Sof(H76B)=Sof(C77A)=Sof(C78A)=Sof(H78A)=Sof(C79A)=Sof(H79A)=
 Sof(C80A)=Sof(H80A)=Sof(C81A)=Sof(H81A)=Sof(C82A)=Sof(H82A)=FVAR(4)
 Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C26B)=Sof(H26B)=Sof(C25B)=Sof(C30B)=
 Sof(H30B)=Sof(C29B)=Sof(H29B)=Sof(C28B)=Sof(H28B)=Sof(C27B)=Sof(H27B)=1-FVAR(5)
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(C30A)=Sof(H30A)=Sof(C29A)=
 Sof(H29A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=Sof(H26A)=FVAR(5)
 Sof(C301)=Sof(H30C)=Sof(H30D)=Sof(H30E)=Sof(C306)=Sof(H306)=Sof(C307)=
 Sof(H307)=Sof(C302)=Sof(C303)=Sof(H303)=Sof(C304)=Sof(H304)=Sof(C305)=
 Sof(H305)=FVAR(6)
 Sof(C308)=Sof(H30F)=Sof(H30G)=Sof(H30H)=Sof(C311)=Sof(H311)=Sof(C312)=
 Sof(H312)=Sof(C313)=Sof(H313)=Sof(C314)=Sof(H314)=Sof(C309)=Sof(C310)=
 Sof(H310)=FVAR(7)
 Sof(C46B)=Sof(H46C)=Sof(H46D)=Sof(C47B)=Sof(C52B)=Sof(H52B)=Sof(C51B)=
 Sof(H51B)=Sof(C50B)=Sof(H50B)=Sof(C49B)=Sof(H49B)=FVAR(8)
 Sof(C27)=Sof(H27)=Sof(C26)=Sof(H26)=Sof(C28)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C48C)=Sof(H48C)=Sof(C46C)=Sof(H46E)=Sof(H46F)=FVAR(9)
 Sof(C48B)=Sof(H48B)=FVAR(10)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C61(H61A,H61B), C3(H3A,H3B), C69(H69A,H69B), C54(H54A,H54B),
 C76(H76A,H76B), C76(H76C,H76D), C31A(H31A,H31B), C24A(H24A,H24B), C39A(H39A,
 H39B), C31B(H31C,H31D), C46A(H46A,H46B), C46B(H46C,H46D), C39B(H39C,H39D),
 C24B(H24C,H24D), C46C(H46E,H46F)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C7(H7), C67(H67), C14(H14), C75(H75), C18(H18), C9(H9),
 C16(H16), C71(H71), C17(H17), C63(H63), C74(H74), C65(H65), C64(H64), C72(H72),
  C73(H73), C66(H66), C56(H56), C58(H58), C60(H60), C57(H57), C59(H59),
 C37A(H37A), C36A(H36A), C35A(H35A), C34A(H34A), C33A(H33A), C78A(H78A),
 C79A(H79A), C80A(H80A), C81A(H81A), C82A(H82A), C30A(H30A), C29A(H29A),
 C28A(H28A), C27A(H27A), C26A(H26A), C45A(H45A), C44A(H44A), C43A(H43A),
 C42A(H42A), C41A(H41A), C37B(H37B), C36B(H36B), C35B(H35B), C34B(H34B),
 C33B(H33B), C52A(H52A), C51A(H51A), C50A(H50A), C49A(H49A), C48A(H48A),
 C52B(H52B), C51B(H51B), C50B(H50B), C49B(H49B), C48B(H48B), C45B(H45B),
 C44B(H44B), C43B(H43B), C42B(H42B), C41B(H41B), C82B(H82B), C81B(H81B),
 C80B(H80B), C79B(H79B), C78B(H78B), C26B(H26B), C30B(H30B), C29B(H29B),
 C28B(H28B), C27B(H27B), C306(H306), C307(H307), C303(H303), C304(H304),
 C305(H305), C311(H311), C312(H312), C313(H313), C314(H314), C310(H310),
 C27(H27), C26(H26), C24(H24), C25(H25), C48C(H48C)
7.c Fitted hexagon refined as free rotating group:
 C32A(C37A,C36A,C35A,C34A,C33A), C77A(C78A,C79A,C80A,C81A,C82A), C25A(C30A,
 C29A,C28A,C27A,C26A), C40A(C45A,C44A,C43A,C42A,C41A), C32B(C37B,C36B,C35B,C34B,
 C33B), C52A(C51A,C50A,C49A,C48A,C47A), C47B(C52B,C51B,C50B,C49B,C48B),
 C40B(C45B,C44B,C43B,C42B,C41B), C77B(C82B,C81B,C80B,C79B,C78B), C26B(C25B,C30B,
 C29B,C28B,C27B), C306(C307,C302,C303,C304,C305), C311(C312,C313,C314,C309,
 C310), C27(C26,C28,C24,C25,C48C)
7.d Idealised Me refined with riding coordinates:
 C301(H30C,H30D,H30E), C308(H30F,H30G,H30H)
7.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C4(H4A,H4B,H4C), C22(H22A,H22B,
 H22C), C13(H13A,H13B,H13C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 144 electrons were 
found in a volume of 568\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[C7H8] per Unit Cell 
which account for 150 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9200
_shelx_hkl_checksum              49958
_shelx_fab_checksum              36892
_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 1.173
_oxdiff_exptl_absorpt_empirical_full_min 0.888