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_1568521
_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 Dy2 K N4 O4 P3, 2(C7 H8)'
_chemical_formula_sum            'C116 H156 Dy2 K N4 O4 P3'
_chemical_formula_weight         2127.45
_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
_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                 119.275(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.3677(14)
_cell_length_b                   23.7878(15)
_cell_length_c                   16.3094(7)
_cell_measurement_reflns_used    36883
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      2.09
_cell_volume                     10615.3(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 (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      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measurement_details
;
 345 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  0.0321
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33310
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.767
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.803
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  0.8535
_exptl_absorpt_correction_T_min  0.5359
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.381
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         13913
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0533P)^2^+33.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10025
_reflns_number_total             13913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ah156_2
_cod_database_code               1568521
_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. Restrained distances
 C43-C42 \\sim C44A-C42
 with sigma of 0.1
 C44A-C42 \\sim C43-C42
 with sigma of 0.01
 C42-C44B \\sim C43-C42
 with sigma of 0.01
3. Rigid bond restraints
 P2, P1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C48B \\sim C49B \\sim C50B \\sim C51B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C44A \\sim C42: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Others
 Fixed Sof: H42(0.5) H42A(0.5) C51A(0.7) H51A(0.7) H51B(0.7) C50A(0.7)
 H50A(0.7) H50B(0.7) C48A(0.7) H48A(0.7) H48B(0.7) C49A(0.7) H49A(0.7)
 H49B(0.7) C44B(0.5) H44A(0.5) H44B(0.5) H44C(0.5) 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) C18B(0.4) H18D(0.4) H18E(0.4) H18F(0.4)
 C17B(0.4) H17D(0.4) H17E(0.4) H17F(0.4) C19B(0.4) H19D(0.4) H19E(0.4)
 H19F(0.4) C49B(0.3) H49C(0.3) H49D(0.3) C48B(0.3) H48C(0.3) H48D(0.3)
 C51B(0.3) H51C(0.3) H51D(0.3) C50B(0.3) H50C(0.3) H50D(0.3) C44A(0.5)
 H44D(0.5) H44E(0.5) H44F(0.5)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C42(H42), C42(H42A), C45(H45)
6.b Secondary CH2 refined with riding coordinates:
 C51A(H51A,H51B), C50A(H50A,H50B), C48A(H48A,H48B), C49A(H49A,H49B), C49B(H49C,
 H49D), C48B(H48C,H48D), C51B(H51C,H51D), C50B(H50C,H50D)
6.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C5(H5), C28(H28), C3(H3), C27(H27), C11(H11), C9(H9), C38(H38),
 C39(H39), C40(H40), C53(H53), C56(H56), C57(H57), C55(H55), C54(H54)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C35(H35A,H35B,H35C), C15(H15A,H15B,H15C), C31(H31A,H31B,
 H31C), C46(H46A,H46B,H46C), C32(H32A,H32B,H32C), C22(H22A,H22B,H22C), C21(H21A,
 H21B,H21C), C47(H47A,H47B,H47C), C43(H43A,H43B,H43C), C34(H34A,H34B,H34C),
 C23(H23A,H23B,H23C), C58(H58A,H58B,H58C), C44B(H44A,H44B,H44C), C17A(H17A,H17B,
 H17C), C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C18B(H18D,H18E,H18F),
 C17B(H17D,H17E,H17F), C19B(H19D,H19E,H19F), C44A(H44D,H44E,H44F)
;
_shelx_res_checksum              75772
_olex2_submission_special_instructions 'No special instructions were received'