Comparison of tetravalent cerium and terbium ions in a conserved, homoleptic imidophosphorane ligand field.
Rice, Natalie T.; Popov, Ivan A.; Russo, Dominic R.; Gompa, Thaige P.; Ramanathan, Arun; Bacsa, John; Batista, Enrique R.; Yang, Ping; La Pierre, Henry S.; Chemical science 11 (2020) 6149–6159; doi:10.1039/d0sc01414a

data_1558079
_publ_section_title
;
 Comparison of tetravalent cerium and terbium ions in a conserved,
 homoleptic imidophosphorane ligand field.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6149
_journal_page_last               6159
_journal_paper_doi               10.1039/d0sc01414a
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C56 H128 Ce N16 P4, K'
_chemical_formula_sum            'C56 H128 Ce K N16 P4'
_chemical_formula_weight         1328.84
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-23
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2020-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                74.835(8)
_cell_angle_beta                 81.559(8)
_cell_angle_gamma                65.275(7)
_cell_formula_units_Z            2
_cell_length_a                   13.160(2)
_cell_length_b                   13.956(3)
_cell_length_c                   23.750(5)
_cell_measurement_reflns_used    9612
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.638
_cell_measurement_theta_min      2.411
_cell_volume                     3820.6(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2  v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            66228
_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         29.130
_diffrn_reflns_theta_min         2.138
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1339 before and 0.0893 after correction. The Ratio of minimum to maximum transmission is 0.8816. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       prism
_exptl_crystal_F_000             1426
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.233
_refine_diff_density_max         1.696
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         20511
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+4.0524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17833
_reflns_number_total             20511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01414a2.cif
_cod_data_source_block           drr-2-023_l
_cod_depositor_comments
;Adding full bibliography for 1558079--1558080.cif.

 Adding full bibliography for 1558079--1558080.cif.
;
_cod_database_code               1558079
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C54-C53
 1.52 with sigma of 0.005
 C39-C38 \\sim C41-C40
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
K1 \\sim K1B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C56) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N13) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(C15) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(K1B) \\sim Ueq, Uanis(K1) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 N16, C53, C54
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 N16, C55, C56
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 N44, C43, C42, N15, C49, C51, C52, C50, C45, C46, C48, C47
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 N13, P3, C40, C41, C38, C39
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N11, C28, C29, N12
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C26, C27, N9, C24, C25
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N7, C20, C23, C22, C21, C14, C15, N8
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Sof(K1B)=1-FVAR(1)
 Sof(K1)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C24(H24A,H24B), C10(H10A,H10B), C5(H5A,H5B), C38(H38A,H38B),
 C53(H53A,H53B), C12(H12A,H12B), C43(H43A,H43B), C40(H40A,H40B), C28(H28A,H28B),
  C55(H55A,H55B), C14(H14A,H14B), C29(H29A,H29B), C15(H15A,H15B), C26(H26A,
 H26B), C42(H42A,H42B)
6.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C35(H35A,H35B,H35C),
 C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C50(H50A,H50B,
 H50C), C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C0AA(H0AA,H0AB,H0AC), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C46(H46A,H46B,H46C), C36(H36A,H36B,H36C), C51(H51A,
 H51B,H51C), C9(H9A,H9B,H9C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C32(H32A,H32B,H32C), C21(H21A,H21B,
 H21C), C18(H18A,H18B,H18C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C19(H19A,
 H19B,H19C), C13(H13A,H13B,H13C), C56(H56A,H56B,H56C), C41(H41A,H41B,H41C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_smtbx_masks_void_probe_radius   0.3
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6283
_shelx_fab_checksum              62011
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id DRR-2-023
_olex2_submission_special_instructions 'No special instructions were received'