Molecular cyclo-P3 complexes of the rare-earth elements via a one-pot reaction and selective reduction
Hauser, Adrian; Münzfeld, Luca; Schlittenhardt, Sören; Köppe, Ralf; Uhlmann, Cedric; Rauska, Ulf-Christian; Ruben, Mario; Roesky, Peter W.; Chemical Science 14 (2023) 2149–2158; doi:10.1039/D2SC06730G

data_1568514
_publ_section_title
;
 Molecular cyclo-P3 complexes of the rare-earth elements via a one-pot
 reaction and selective reduction
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2149
_journal_page_last               2158
_journal_paper_doi               10.1039/D2SC06730G
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C55 H78 N2 O3 Sm'
_chemical_formula_sum            'C55 H78 N2 O3 Sm'
_chemical_formula_weight         965.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.465(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5817(8)
_cell_length_b                   14.3505(6)
_cell_length_c                   13.9019(8)
_cell_measurement_reflns_used    93777
_cell_measurement_temperature    110
_cell_measurement_theta_max      31.62
_cell_measurement_theta_min      2.17
_cell_volume                     2425.6(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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_temperature      110.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
 1325 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65099
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.822
_diffrn_reflns_theta_min         2.166
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.8398
_exptl_absorpt_correction_T_min  0.3416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.072
_refine_diff_density_max         2.264
_refine_diff_density_min         -2.964
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details
;
 Flack x determined using 4973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         14294
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+13.6182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                11804
_reflns_number_total             14294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ah108_3
_cod_database_code               1568514
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.779
_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
 C34B-C33B \\sim C35A-C33B
 with sigma of 0.01
 C34B-C33B \\sim C35B-C33B
 with sigma of 0.01
 C30-C29 \\sim C33A-C25
 with sigma of 0.01
 C33B-C25 \\sim C30-C29
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C33A \\sim C34A \\sim C35A: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C33B \\sim C34B \\sim C35B: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C34B(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C33B(0.5) H33B(0.5)
 C35B(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C35A(0.5) H35D(0.5) H35E(0.5)
 H35F(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C33A(0.5) H33A(0.5)
5.a Ternary CH refined with riding coordinates:
 C42(H42), C45(H45), C33B(H33B), C30(H30), C33A(H33A)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C53(H53A,H53B), C49(H49A,H49B), C48(H48A,H48B), C50(H50A,
 H50B), C54(H54A,H54B), C55(H55A,H55B), C52(H52A,H52B)
5.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C3(H3), C26(H26), C39(H39), C40(H40), C9(H9), C11(H11), C28(H28),
 C38(H38), C5(H5)
5.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C43(H43A,H43B,
 H43C), C46(H46A,H46B,H46C), C18(H18A,H18B,H18C), C34B(H34A,H34B,H34C),
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C15(H15A,H15B,
 H15C), C14(H14A,H14B,H14C), C44(H44A,H44B,H44C), C32(H32A,H32B,H32C), C31(H31A,
 H31B,H31C), C35B(H35A,H35B,H35C), C35A(H35D,H35E,H35F), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              86206
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'