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_1568520
_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         'C102 H140 K N4 O4 P3 Sm2, 2(C7 H8)'
_chemical_formula_sum            'C116 H156 K N4 O4 P3 Sm2'
_chemical_formula_weight         2103.15
_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             2022-04-15
_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                 119.805(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6860(19)
_cell_length_b                   23.6758(8)
_cell_length_c                   16.4497(9)
_cell_measurement_reflns_used    43585
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.09
_cell_volume                     10708.1(10)
_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 0.806
_diffrn_measurement_details
;
 480 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_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54911
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.795
_diffrn_reflns_theta_min         2.092
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  0.9236
_exptl_absorpt_correction_T_min  0.5403
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.029
_refine_diff_density_min         -1.943
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14738
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0502P)^2^+96.1343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8998
_reflns_number_total             14738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ah159_2
_cod_database_code               1568520
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.795
_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
 C48B-C49B \\sim C51A-C50A \\sim C49B-C50B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2B \\sim C48B \\sim C49B \\sim C50B \\sim C51B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C49A \\sim C48A \\sim O2A \\sim C51A \\sim C50A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C45: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: O2A(0.75) C50A(0.75) H50A(0.75) H50B(0.75) C49A(0.75) H49A(0.75)
 H49B(0.75) C17A(0.6) H17A(0.6) H17B(0.6) H17C(0.6) C18A(0.6) H18A(0.6)
 H18B(0.6) H18C(0.6) C19A(0.6) H19A(0.6) H19B(0.6) H19C(0.6) C19B(0.4)
 H19D(0.4) H19E(0.4) H19F(0.4) C17B(0.4) H17D(0.4) H17E(0.4) H17F(0.4)
 C18B(0.4) H18D(0.4) H18E(0.4) H18F(0.4) C48A(0.75) H48A(0.75) H48B(0.75)
 C48B(0.25) H48C(0.25) H48D(0.25) C50B(0.25) H50C(0.25) H50D(0.25) C49B(0.25)
 H49C(0.25) H49D(0.25) O2B(0.25) C51A(0.75) H51A(0.75) H51B(0.75) C51B(0.25)
 H51C(0.25) H51D(0.25) C47A(0.6) H47A(0.6) H47B(0.6) H47C(0.6) C47B(0.4)
 H47D(0.4) H47E(0.4) H47F(0.4)
5.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C45(H45), C42(H42)
5.b Secondary CH2 refined with riding coordinates:
 C50A(H50A,H50B), C49A(H49A,H49B), C48A(H48A,H48B), C48B(H48C,H48D), C50B(H50C,
 H50D), C49B(H49C,H49D), C51A(H51A,H51B), C51B(H51C,H51D)
5.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C28(H28), C3(H3), C5(H5), C27(H27), C11(H11), C9(H9), C38(H38),
 C53(H53), C40(H40), C39(H39), C57(H57), C54(H54), C55(H55), C56(H56)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C15(H15A,H15B,
 H15C), C31(H31A,H31B,H31C), C43(H43A,H43B,H43C), C22(H22A,H22B,H22C), C44(H44A,
 H44B,H44C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C),
 C58(H58A,H58B,H58C), C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C19A(H19A,
 H19B,H19C), C19B(H19D,H19E,H19F), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F),
 C46(H46A,H46B,H46C), C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F)
;
_shelx_res_checksum              91784
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'