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_1558080
_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_absolute_configuration ad
_chemical_formula_moiety         'C56 H128 Ce N16 P4'
_chemical_formula_sum            'C56 H128 Ce N16 P4'
_chemical_formula_weight         1289.74
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-12
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3726(10)
_cell_length_b                   13.3726(10)
_cell_length_c                   21.0511(17)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.25
_cell_measurement_theta_min      3.05
_cell_volume                     3764.5(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2  v2014.1-1 (Bruker, 2014)'
_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 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            44868
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.303
_diffrn_reflns_theta_min         2.896
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.5676
_exptl_absorpt_correction_T_min  0.5287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2016/2. (Krause, L. et al, 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       prism
_exptl_crystal_F_000             1388
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.301
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.189(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         9035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0424P)^2^+1.5350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.957
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                8979
_reflns_number_total             9035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01414a2.cif
_cod_data_source_block           drr-2-018_l_sq
_cod_depositor_comments
;Adding full bibliography for 1558079--1558080.cif.

 Adding full bibliography for 1558079--1558080.cif.
;
_cod_original_cell_volume        3764.5(6)
_cod_database_code               1558080
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.811(8)
 0.189(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C2(H2A,H2B), C1(H1A,H1B), C13(H13A,H13B)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   0.5
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16681
_shelx_fab_checksum              21699
_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-2-018
_olex2_submission_special_instructions 'No special instructions were received'