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_7705690
_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 H155 Ce N18 P3, [+ solvents]'
_chemical_formula_sum            'C89 H168 Ce N18 P3'
_chemical_formula_weight         1723.43
_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   mixed
_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                81.638(5)
_cell_angle_beta                 88.524(6)
_cell_angle_gamma                61.054(4)
_cell_formula_units_Z            2
_cell_length_a                   16.104(2)
_cell_length_b                   16.452(2)
_cell_length_c                   20.980(3)
_cell_measurement_reflns_used    9098
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.93
_cell_measurement_theta_min      2.33
_cell_volume                     4806.0(11)
_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(1)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            148026
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.005
_diffrn_reflns_theta_min         2.248
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.05
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.5647
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0760 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.8994.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       prism
_exptl_crystal_F_000             1862
_exptl_crystal_recrystallization_method
'The material was recrystallised from pentane'
_exptl_crystal_size_max          0.591
_exptl_crystal_size_mid          0.351
_exptl_crystal_size_min          0.342
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00048(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         30201
_refine_ls_number_restraints     1264
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0461P)^2^+3.9232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25307
_reflns_number_total             30201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03472j2.cif
_cod_data_source_block           1-ce
_cod_depositor_comments
'Adding full bibliography for 7705688--7705690.cif.'
_cod_database_code               7705690
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P2-N5_11 \\sim P2-N5_12 \\sim P2-N5_9 \\sim P2-N5_14
 with sigma of 0.004
 P1-N5 \\sim P1-N5_3
 with sigma of 0.002
 P1-N5_2 \\sim P1-N5_8
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C21_8) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C22_11) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(N5_2) = Uanis(N5_8)
Uanis(N5_12) = Uanis(N5_11)
Uanis(C20_3) = Uanis(C20)
Uanis(N5) = Uanis(N5_3)
Uanis(C19_3) = Uanis(C19)
Uanis(N5_14) = Uanis(N5_9)
Uanis(C19_2) = Uanis(C19_8)
4. Rigid body (RIGU) restrains
 C19_1, C20_1, C21_1, C22_1, C23_1, N5_1
 C19_2, C20_2, C21_2, C22_2, C23_2, N5_2
 C19_3, C20_3, C21_3, C22_3, C23_3, N5_3
 C19_4, C20_4, C21_4, C22_4, C23_4, N5_4
 C19_7, C20_7, C21_7, C22_7, C23_7, N5_7
 C19_8, C20_8, C21_8, C22_8, C23_8, N5_8
 C19_9, C20_9, C21_9, C22_9, C23_9, N5_9
 C19_10, C20_10, C21_10, C22_10, C23_10, N5_10
 C19_11, C20_11, C21_11, C22_11, C23_11, N5_11
 C19_12, C20_12, C21_12, C22_12, C23_12, N5_12
 C19_13, C20_13, C21_13, C22_13, C23_13, N5_13
 C19_14, C20_14, C21_14, C22_14, C23_14, N5_14
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0004
 P3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P1, N5_1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P1, N5_8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P3, N5_4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P2, N5_14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N5_12, P2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P1, N5_3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P1, N5_2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{C19_2, C20_2, C21_2, C22_2, C23_2, N5_2}
{C19_3, C20_3, C21_3, C22_3, C23_3, N5_3}
{C19_4, C20_4, C21_4, C22_4, C23_4, N5_4}
{C19_7, C20_7, C21_7, C22_7, C23_7, N5_7}
{C19_8, C20_8, C21_8, C22_8, C23_8, N5_8}
{C19_9, C20_9, C21_9, C22_9, C23_9, N5_9}
{C19_10, C20_10, C21_10, C22_10, C23_10, N5_10}
{C19_11, C20_11, C21_11, C22_11, C23_11, N5_11}
{C19_12, C20_12, C21_12, C22_12, C23_12, N5_12}
{C19_13, C20_13, C21_13, C22_13, C23_13, N5_13}
{C19_14, C20_14, C21_14, C22_14, C23_14, N5_14}
as
{C19_1, C20_1, C21_1, C22_1, C23_1, N5_1} sigma for 1-2: 0.002 1-3: 0.004
6. Others
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=1-
 FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=
 FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=1-
 FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=
 FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=1-
 FVAR(3)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=
 FVAR(3)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=1-
 FVAR(4)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(N5)=
 FVAR(4)
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:
 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), 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),
 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), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
;
_smtbx_masks_void_probe_radius   0.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7739
_shelx_fab_checksum              20112
_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'