Coinage metal tris(dialkylamido)imidophosphorane complexes as transmetallation reagents for cerium complexes.
Aguirre Quintana, Luis M.; Jiang, Ningxin; Bacsa, John; La Pierre, Henry S.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5420–5423; doi:10.1039/d0dt00842g

data_7703924
_publ_section_title
;
 Coinage metal tris(dialkylamido)imidophosphorane complexes as
 transmetallation reagents for cerium complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5420
_journal_page_last               5423
_journal_paper_doi               10.1039/d0dt00842g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '4(C56 H128 Ag4 N16 P4), 4(C4 H8 O)'
_chemical_formula_sum            'C240 H544 Ag16 N64 O4 P16'
_chemical_formula_weight         6612.80
_chemical_name_systematic        Ag4(PN)4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.291(2)
_cell_length_b                   17.4258(19)
_cell_length_c                   26.727(3)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.22
_cell_volume                     8518.8(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            73513
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         2.338
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.9826
_exptl_absorpt_correction_T_min  0.7261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1235 before and 0.0912 after correction.
The Ratio of minimum to maximum transmission is 0.7390.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       prism
_exptl_crystal_F_000             3456
_exptl_crystal_preparation       N.A.
_exptl_crystal_recrystallization_method N.A.
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.949
_refine_diff_density_min         -1.714
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         9789
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0803P)^2^+78.7477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.2138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6912
_reflns_number_total             9789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00842g2.cif
_cod_data_source_block           a594_0ma
_cod_depositor_comments
'Adding full bibliography for 7703924--7703927.cif.'
_cod_database_code               7703924
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29_$1-C29
 1.34 with sigma of 0.005
 C2B-C1B \\sim C2A-C1A
 with sigma of 0.005
 C30A-C29_$1 \\sim C30B-C29_$1
 with sigma of 0.002
 O1-C30A_$1 \\sim O1-C30B_$1
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C14A) \\sim Ueq, Uanis(C14B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C2A) \\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(N6A) \\sim Ueq, Uanis(N6B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C30B) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N6A) = Uanis(N6B)
Uanis(C16A) = Uanis(C16B)
Uanis(C15A) = Uanis(C15B)
Uanis(C4B) = Uanis(C4A)
Uanis(C3A) = Uanis(C3B)
Uanis(N2A) = Uanis(N2B)
Uanis(C2A) = Uanis(C2B)
Uanis(C17B) = Uanis(C17A)
Uanis(C11A) = Uanis(C11B)
Uanis(C14A) = Uanis(C14B)
Uanis(C12A) = Uanis(C12B)
Uanis(C13A) = Uanis(C13B)
Uanis(C1B) = Uanis(C1A)
Uanis(C30A) = Uanis(C30B)
4. Same fragment restrains
{C2B, N2B, C3B, C4B} sigma for 1-2: 0.005, 1-3: 0.01
as
{C2A, N2A, C3A, C4A}
{C11B, C12B, C13B} sigma for 1-2: 0.005, 1-3: 0.01
as
{C11A, C12A, C13A}
{N6B, C15B, C16B, C17B, C18B} sigma for 1-2: 0.005, 1-3: 0.01
as
{N6A, C15A, C16A, C17A, C18A}
5. Others
 Sof(N6B)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16C)=
 Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=1-FVAR(1)
 Sof(N6A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(N2B)=
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=1-FVAR(2)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(N2A)=
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(2)
 Sof(C11B)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13B)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(3)
 Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(H29C)=Sof(H29D)=1-FVAR(4)
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30C)=Sof(H30D)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C23(H23A,H23B), C24(H24A,H24B), C2A(H2AA,H2AB),
 C3A(H3AA,H3AB), C16A(H16A,H16B), C17A(H17A,H17B), C2B(H2BA,H2BB), C3B(H3BA,
 H3BB), C16B(H16C,H16D), C17B(H17C,H17D), C30B(H30A,H30B), C29(H29C,H29D),
 C29(H29A,H29B), C30A(H30C,H30D)
6.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC),
 C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C15A(H15A,
 H15B,H15C), C18A(H18A,H18B,H18C), C1B(H1BA,H1BB,H1BC), C4B(H4BA,H4BB,H4BC),
 C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F), C18B(H18D,H18E,H18F)
;
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id 'Ag4(PN)4 THF'
_olex2_submission_special_instructions 'No special instructions were received'