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_7703925
_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         'C60 H120 Ag4 N16 P4'
_chemical_formula_sum            'C60 H120 Ag4 N16 P4'
_chemical_formula_weight         1621.07
_chemical_name_systematic        Ag4N16P4C60H120
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.06.07 svn.r3419 for OlexSys, GUI svn.r5353)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.657(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.417(4)
_cell_length_b                   15.104(2)
_cell_length_c                   40.405(8)
_cell_measurement_reflns_used    9363
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.567
_cell_measurement_theta_min      2.436
_cell_volume                     14936(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_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  0.0658
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            52846
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.618
_diffrn_reflns_theta_min         2.192
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1493 before and 0.0876 after correction. The Ratio of minimum to maximum transmission is 0.7262. 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    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             6720
_exptl_crystal_preparation       N.A.
_exptl_crystal_recrystallization_method N.A.
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         17175
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+60.6437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14271
_reflns_number_total             17175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00842g2.cif
_cod_data_source_block           a668_0m
_cod_depositor_comments
'Adding full bibliography for 7703924--7703927.cif.'
_cod_original_cell_volume        14935(5)
_cod_database_code               7703925
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C36A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(C39A) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C40B) \\sim Ueq, Uanis(C39B) \\sim Ueq, Uanis(C38B) \\sim Ueq,
Uanis(C37B) \\sim Ueq, Uanis(C36B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(N7A) = Uanis(N7B)
Uanis(C25A) = Uanis(C25B)
Uanis(C24A) = Uanis(C24B)
Uanis(C23A) = Uanis(C23B)
Uanis(C22A) = Uanis(C22B)
Uanis(C21A) = Uanis(C21B)
Uanis(N10A) = Uanis(N10B)
Uanis(C31A) = Uanis(C31B)
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
Uanis(C34A) = Uanis(C34B)
Uanis(C35A) = Uanis(C35B)
Uanis(N11A) = Uanis(N11B)
Uanis(N12A) = Uanis(N12B)
Uanis(C45A) = Uanis(C45B)
Uanis(C44A) = Uanis(C44B)
Uanis(C43A) = Uanis(C43B)
Uanis(C42A) = Uanis(C42B)
Uanis(C41A) = Uanis(C41B)
3. Same fragment restrains
{N7B, C21B, C22B, C23B, C24B, C25B} sigma for 1-2: 0.002, 1-3: 0.004
as
{N7A, C21A, C22A, C23A, C24A, C25A}
{N10B, C31B, C32B, C33B, C34B, C35B} sigma for 1-2: 0.002, 1-3: 0.004
as
{N10A, C31A, C32A, C33A, C34A, C35A}
{N12B, C41B} sigma for 1-2: 0.002, 1-3: 0.004
as
{N12A, C45A}
{N11B, C36B, C37B, C38B, C39B, C40B} sigma for 1-2: 0.002, 1-3: 0.004
as
{N11A, C36A, C37A, C38A, C39A, C40A}
4. Others
 Sof(N7B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=
 Sof(H25C)=Sof(H25D)=1-FVAR(1)
 Sof(N7A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=FVAR(1)
 Sof(N10B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(C35B)=
 Sof(H35C)=Sof(H35D)=Sof(N11A)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=
 Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=
 Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(2)
 Sof(N10A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(C35A)=
 Sof(H35A)=Sof(H35B)=Sof(N11B)=Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(C37B)=
 Sof(H37A)=Sof(H37B)=Sof(C38B)=Sof(H38A)=Sof(H38B)=Sof(C39B)=Sof(H39A)=
 Sof(H39B)=Sof(C40B)=Sof(H40A)=Sof(H40B)=FVAR(2)
 Sof(N12B)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=
 Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=Sof(C45B)=
 Sof(H45C)=Sof(H45D)=1-FVAR(3)
 Sof(N12A)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=
 Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C41A)=
 Sof(H41A)=Sof(H41B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), 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), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 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), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,H23B), C24A(H24A,
 H24B), C25A(H25A,H25B), C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,H33B),
 C34A(H34A,H34B), C35A(H35A,H35B), C36B(H36A,H36B), C37B(H37A,H37B), C38B(H38A,
 H38B), C39B(H39A,H39B), C40B(H40A,H40B), C45A(H45A,H45B), C44A(H44A,H44B),
 C43A(H43A,H43B), C42A(H42A,H42B), C41A(H41A,H41B), C21B(H21C,H21D), C22B(H22C,
 H22D), C23B(H23C,H23D), C24B(H24C,H24D), C25B(H25C,H25D), C31B(H31C,H31D),
 C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D), C35B(H35C,H35D), C36A(H36C,
 H36D), C37A(H37C,H37D), C38A(H38C,H38D), C39A(H39C,H39D), C40A(H40C,H40D),
 C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,H43D), C44B(H44C,H44D), C45B(H45C,
 H45D)
;
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id Ag4(Pipen)4
_olex2_submission_special_instructions 'No special instructions were received'