Homoleptic cerium tris(dialkylamido)imidophosphorane guanidinate complexes.
Aguirre Quintana, Luis M.; Jiang, Ningxin; Bacsa, John; La Pierre, Henry S.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14908–14913; doi:10.1039/d0dt03472j

data_7705689
_publ_section_title
;
 Homoleptic cerium tris(dialkylamido)imidophosphorane guanidinate
 complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14908
_journal_page_last               14913
_journal_paper_doi               10.1039/d0dt03472j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C84 H158 Ce N18 P3, C24 H20 B, 1.5(C5H12)'
_chemical_formula_sum            'C123 H214 B Ce N18 P3'
_chemical_formula_weight         2188.95
_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
_audit_creation_date             2020-10-12
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2020-10-12 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                95.893(7)
_cell_angle_beta                 99.060(7)
_cell_angle_gamma                91.156(7)
_cell_formula_units_Z            2
_cell_length_a                   13.438(2)
_cell_length_b                   19.340(3)
_cell_length_c                   22.773(4)
_cell_measurement_reflns_used    9561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.20
_cell_volume                     5809.8(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2013)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
; 
 Bruker D8 VENTURE diffractometer with a PHOTON-2 detector.
;
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            120674
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.708
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.065
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1074 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.9336.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       needle
_exptl_crystal_F_000             2372
_exptl_crystal_recrystallization_method
'The material was recrystallised from pentane'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.077
_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     1205
_refine_ls_number_reflns         29760
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+4.0720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24344
_reflns_number_total             29760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03472j2.cif
_cod_data_source_block           2-ce
_cod_depositor_comments
'Adding full bibliography for 7705688--7705690.cif.'
_cod_original_cell_volume        5809.9(17)
_cod_database_code               7705689
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 P3-N18B \\sim P3-N18A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(N18B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.004
Uanis(N18A) = Uanis(N18B)
Uanis(C80A) = Uanis(C80B)
Uanis(C81A) = Uanis(C81B)
Uanis(C83A) = Uanis(C83B)
Uanis(C84A) = Uanis(C84B)
4. Rigid body (RIGU) restrains
 P3, N18B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 N18A, C80A, H80A, H80B, C81A, H81A, H81B, C82A, H82A, H82B, C83A, H83A, H83B,
 C84A, H84A, H84B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N18B, C80B, C81B, C82B, C83B, C84B} sigma for 1-2: 0.002, 1-3: 0.004
as in
{N18A, C80A, C81A, C82A, C83A, C84A}
6. Others
 Sof(N18B)=Sof(C80B)=Sof(H80C)=Sof(H80D)=Sof(C81B)=Sof(H81C)=Sof(H81D)=
 Sof(C82B)=Sof(H82C)=Sof(H82D)=Sof(C83B)=Sof(H83C)=Sof(H83D)=Sof(C84B)=
 Sof(H84C)=Sof(H84D)=1-FVAR(1)
 Sof(N18A)=Sof(C80A)=Sof(H80A)=Sof(H80B)=Sof(C81A)=Sof(H81A)=Sof(H81B)=
 Sof(C82A)=Sof(H82A)=Sof(H82B)=Sof(C83A)=Sof(H83A)=Sof(H83B)=Sof(C84A)=
 Sof(H84A)=Sof(H84B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C30(H30), C36(H36), C58(H58), C64(H64)
7.b Secondary CH2 refined with riding coordinates:
 C80A(H80A,H80B), C81A(H81A,H81B), C82A(H82A,H82B), C83A(H83A,H83B), C84A(H84A,
 H84B), C80B(H80C,H80D), C81B(H81C,H81D), C82B(H82C,H82D), C83B(H83C,H83D),
 C84B(H84C,H84D), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,
 H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C59(H59A,H59B), C60(H60A,
 H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B)
7.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N15(H15), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92),
 C93(H93), C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100),
 C101(H101), C102(H102), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108)
;
_smtbx_masks_void_probe_radius   0.3
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61688
_shelx_fab_checksum              33900
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone'
_olex2_submission_special_instructions 'No special instructions were received'