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_1568516
_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 H82 B N2 O3 Y'
_chemical_formula_sum            'C55 H82 B N2 O3 Y'
_chemical_formula_weight         918.94
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.698(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7490(9)
_cell_length_b                   14.0841(6)
_cell_length_c                   26.9502(17)
_cell_measurement_reflns_used    27662
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.13
_cell_measurement_theta_min      1.97
_cell_volume                     5158.7(5)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_details
;
 419 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30771
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.338
_diffrn_reflns_theta_min         1.972
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.8864
_exptl_absorpt_correction_T_min  0.5192
_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, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         13149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+7.3463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9559
_reflns_number_total             13149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ah161
_cod_database_code               1568516
_shelx_shelxl_version_number     2018/3
_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.a Ternary CH refined with riding coordinates:
 C42(H42), C30(H30), C45(H45), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C51(H51A,
 H51B), C52(H52A,H52B), C49(H49A,H49B), C48(H48A,H48B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C8(H8), C2(H2), C38(H38), C26(H26), C27(H27), C28(H28),
 C39(H39), C40(H40)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C47(H47A,H47B,H47C), C23(H23A,H23B,
 H23C), C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C31(H31A,
 H31B,H31C), C22(H22A,H22B,H22C), C46(H46A,H46B,H46C), C44(H44A,H44B,H44C),
 C19(H19A,H19B,H19C), C35(H35A,H35B,H35C), C18(H18A,H18B,H18C), C43(H43A,H43B,
 H43C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              67767
_olex2_submission_special_instructions 'No special instructions were received'