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_7059564
_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
'Al C36 F46 O3, C45 H63 Ag B3 N3 P3, 1[CH2Cl2]'
_chemical_formula_sum            'C82 H65 Ag Al B3 Cl2 F46 N3 O3 P3'
_chemical_formula_weight         2345.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 90.4893(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.41518(14)
_cell_length_b                   19.8618(3)
_cell_length_c                   42.3218(5)
_cell_measurement_reflns_used    50885
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      27.5160
_cell_measurement_theta_min      3.5440
_cell_volume                     9595.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9851
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     43.00  98.00   0.50   20.00    --   20.57 178.00-150.00  110
  2  \w     69.00  98.00   0.50   20.00    --   20.57 178.00 -30.00   58
  3  \w    -46.00  64.00   0.50   20.00    --   20.57 -19.00-150.00  220
  4  \w    -27.00  61.00   0.50   20.00    --   20.57 -93.00 171.00  176
  5  \w    -99.00 -34.00   0.50   20.00    --  -20.73 178.00 -90.00  130
  6  \w    -93.00   7.00   0.50   20.00    --  -20.73 -38.00   0.00  200
  7  \w    -90.00   1.00   0.50   20.00    --  -20.73 -57.00 150.00  182
  8  \w    -93.00   7.00   0.50   20.00    --  -20.73 -38.00-150.00  200
  9  \w    -92.00  11.00   0.50   20.00    --  -20.73 -77.00 -60.00  206
 10  \w    -61.00 -26.00   0.50   20.00    --  -20.73  93.00 -76.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0038955000
_diffrn_orient_matrix_UB_12      -0.0224338000
_diffrn_orient_matrix_UB_13      -0.0129873000
_diffrn_orient_matrix_UB_21      0.0271534000
_diffrn_orient_matrix_UB_22      -0.0243447000
_diffrn_orient_matrix_UB_23      0.0099014000
_diffrn_orient_matrix_UB_31      -0.0557387000
_diffrn_orient_matrix_UB_32      -0.0134430000
_diffrn_orient_matrix_UB_33      0.0037485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            146206
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.154
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.37b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.624
_exptl_crystal_description       needle
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         21220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0490P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15636
_reflns_number_total             21220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01679a2.cif
_cod_data_source_block           hulk218
_cod_depositor_comments
'Adding full bibliography for 7059562--7059565.cif.'
_cod_database_code               7059564
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula
'Ag (C15 H21 B P N )3 Al O3 C36 F46 (C H2 Cl2)0.45'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.776
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66656
_shelx_fab_checksum              374
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.032
_oxdiff_exptl_absorpt_empirical_full_min 0.490