A new family of silver(i) complexes stabilised by the phosphanylborane (C6H5)2PBH2·N(CH3)3
Elsayed Moussa, Mehdi; Marquardt, Christian; Hegen, Oliver; Seidl, Michael; Scheer, Manfred; New Journal of Chemistry 45 (2021) 14916–14919; doi:10.1039/D0NJ01679A

data_7059563
_publ_section_title
;
 A new family of silver(i) complexes stabilised by the phosphanylborane
 (C6H5)2PBH2&#x00B7;N(CH3)3
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14916
_journal_page_last               14919
_journal_paper_doi               10.1039/D0NJ01679A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C30 H42 Ag B2 N2 P2, Al C36 F46 O3'
_chemical_formula_sum            'C66 H42 Ag Al B2 F46 N2 O3 P2'
_chemical_formula_weight         2003.42
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-30
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-04-03 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                66.0358(15)
_cell_angle_beta                 88.8395(14)
_cell_angle_gamma                73.5586(17)
_cell_formula_units_Z            2
_cell_length_a                   11.3066(2)
_cell_length_b                   17.6908(3)
_cell_length_c                   21.6344(3)
_cell_measurement_reflns_used    19058
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      72.8370
_cell_measurement_theta_min      4.0780
_cell_volume                     3770.45(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -98.00   -2.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.6172  125.0000 -180.0000 192

  2 omega    7.00  118.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.6172   37.0000  120.0000 222

  3 omega    9.00  123.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.6172   77.0000  -30.0000 228

  4 omega   31.00  128.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -61.0000   60.0000 194

  5 omega   29.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942 -111.0000   30.0000 172

  6 omega   74.00  110.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942 -111.0000  -60.0000 72

  7 omega   16.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942    0.0000    0.0000 284

  8 omega   28.00  114.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942 -111.0000 -150.0000 172

  9 omega   28.00   67.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -30.0000    0.0000 78

 10 omega   27.00   61.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -30.0000   60.0000 68

 11 omega   41.00  109.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -94.0000   60.0000 136

 12 omega   30.00   56.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942 -111.0000  -60.0000 52

 13 omega   28.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -30.0000  150.0000 82

 14 omega   32.00   66.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -30.0000   90.0000 68

 15 omega   27.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -30.0000  -30.0000 74

 16 omega   33.00  138.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942  -61.0000 -150.0000 210

 17 omega -124.00  -79.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.6172  -99.0000  -30.0000 90

 18 omega  -20.00   83.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.6172  -99.0000   30.0000 206

 19 omega    7.00  118.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.6172   37.0000 -120.0000 222

 20 omega   70.00   95.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1942   30.0000   90.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0422828000
_diffrn_orient_matrix_UB_12      0.0693340000
_diffrn_orient_matrix_UB_13      0.0113081000
_diffrn_orient_matrix_UB_21      0.1273179000
_diffrn_orient_matrix_UB_22      -0.0318098000
_diffrn_orient_matrix_UB_23      -0.0228977000
_diffrn_orient_matrix_UB_31      -0.0492189000
_diffrn_orient_matrix_UB_32      0.0645438000
_diffrn_orient_matrix_UB_33      -0.0741083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27960
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.962
_diffrn_reflns_theta_min         4.101
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.2068
_exptl_crystal_size_mid          0.1195
_exptl_crystal_size_min          0.0995
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         14497
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0313P)^2^+0.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13677
_reflns_number_total             14497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01679a2.cif
_cod_data_source_block           cm429edrabs
_cod_depositor_comments
'Adding full bibliography for 7059562--7059565.cif.'
_cod_database_code               7059563
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag1 C66 H42 N2 B2 P2 Al1 O3 F46'
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1B-C10 \\sim P1A-C10 \\sim P1A-C4A \\sim P1B-C4B
 with sigma of 0.04
 C7B-C8B \\sim C8B-C9B \\sim C9B-C4B \\sim C4B-C5B \\sim C5B-C6B \\sim C6B-C7B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C2B \\sim N1B \\sim C3B \\sim C1B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.9A
C7B \\sim C8B \\sim C9B \\sim C4B \\sim C5B \\sim C6B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(B1B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Ag1B)=Sof(P1B)=Sof(N1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(B1B)=
 Sof(H1BD)=Sof(H1BE)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=
 Sof(C4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(Ag1A)=Sof(P1A)=Sof(N1A)=Sof(C4A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C5A)=Sof(H5A)=Sof(B1A)=Sof(C9A)=
 Sof(H9A)=Sof(C7A)=Sof(H7A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C6A)=
 Sof(H6A)=Sof(C8A)=Sof(H8A)=Sof(H1AD)=Sof(H1AE)=FVAR(1)
 Fixed Uiso: H17A(0.095) H17B(0.095) H17C(0.095)
5.a Secondary CH2 refined with riding coordinates:
 B1B(H1BD,H1BE)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C15(H15), C11(H11), C22(H22), C23(H23), C70(H70), C13(H13),
 C26(H26), C12(H12), C21(H21), C30(H30), C20(H20), C5A(H5A), C9A(H9A), C7A(H7A),
  C27(H27), C28(H28), C6A(H6A), C29(H29), C8A(H8A), C7B(H7B), C8B(H8B),
 C9B(H9B), C5B(H5B), C6B(H6B)
5.c Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C18(H18A,H18B,
 H18C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C1B(H1BA,H1BB,H1BC), C3B(H3BA,
 H3BB,H3BC), C2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              97865
_olex2_submission_special_instructions 'No special instructions were received'