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_7703927
_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 H129 Cu4 N16 P4), 4(C4 H8 O)'
_chemical_formula_sum            'C240 H548 Cu16 N64 O4 P16'
_chemical_formula_weight         5907.55
_chemical_name_systematic        'Cu4(PN)4 THF'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-17
_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                 93.561(7)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   13.463(2)
_cell_length_b                   22.899(4)
_cell_length_c                   24.461(4)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.262
_cell_measurement_theta_min      2.332
_cell_volume                     7527(2)
_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)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.988
_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  0.0756
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            74391
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.379
_diffrn_reflns_theta_min         2.337
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_correction_T_min  0.8048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1345 before and 0.0763 after correction. The Ratio of minimum to maximum transmission is 0.8284. 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    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             3172
_exptl_crystal_preparation       N.A.
_exptl_crystal_recrystallization_method N.A.
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         18628
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0294P)^2^+9.8045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13274
_reflns_number_total             18628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00842g2.cif
_cod_data_source_block           a595_0m
_cod_depositor_comments
'Adding full bibliography for 7703924--7703927.cif.'
_cod_original_cell_volume        7526(2)
_cod_database_code               7703927
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59A-C58A \\sim C59B-C58B
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59B) \\sim Ueq, Uanis(C58B)
\\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C59A) = Uanis(C59B)
Uanis(C58A) = Uanis(C58B)
4. Others
 Sof(H60C)=Sof(H60D)=Sof(H57C)=Sof(H57D)=Sof(C59B)=Sof(H59A)=Sof(H59B)=
 Sof(C58B)=Sof(H58A)=Sof(H58B)=1-FVAR(1)
 Sof(H60B)=Sof(H60A)=Sof(H57A)=Sof(H57B)=Sof(C59A)=Sof(H59C)=Sof(H59D)=
 Sof(C58A)=Sof(H58C)=Sof(H58D)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C30(H30A,H30B), C10(H10A,H10B), C9(H9A,H9B), C16(H16A,H16B),
 C2(H2A,H2B), C52(H52A,H52B), C23(H23A,H23B), C22(H22A,H22B), C44(H44A,H44B),
 C45(H45A,H45B), C51(H51A,H51B), C17(H17A,H17B), C37(H37A,H37B), C31(H31A,H31B),
  C38(H38A,H38B), C60(H60C,H60D), C60(H60B,H60A), C57(H57C,H57D), C57(H57A,
 H57B), C59B(H59A,H59B), C58B(H58A,H58B), C59A(H59C,H59D), C58A(H58C,H58D)
5.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C55(H55A,
 H55B,H55C), C13(H13A,H13B,H13C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C),
 C26(H26A,H26B,H26C), C6(H6A,H6B,H6C), C01I(H01A,H01B,H01C), C29(H29A,H29B,
 H29C), C40(H40A,H40B,H40C), C21(H21A,H21B,H21C), C8(H8A,H8B,H8C), C4(H4A,H4B,
 H4C), C1(H1A,H1B,H1C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C46(H46A,H46B,
 H46C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C50(H50A,
 H50B,H50C), C18(H18A,H18B,H18C), C49(H49A,H49B,H49C), C41(H41A,H41B,H41C),
 C32(H32A,H32B,H32C), C15(H15A,H15B,H15C)
;
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id 'Cu4(PN)4 THF'
_olex2_submission_special_instructions 'No special instructions were received'