Silver halide complexes of a borane/bis(phosphine) ligand.
Cao, Yihan; Shih, Wei-Chun; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9959–9961; doi:10.1039/c9dt02100k

data_7700273
_publ_section_title
;
 Silver halide complexes of a borane/bis(phosphine) ligand.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9959
_journal_page_last               9961
_journal_paper_doi               10.1039/c9dt02100k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H82 Ag2 B2 F2 P4, C7 H8'
_chemical_formula_sum            'C67 H90 Ag2 B2 F2 P4'
_chemical_formula_weight         1294.62
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-13 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.983(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.169(3)
_cell_length_b                   24.543(5)
_cell_length_c                   19.555(4)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.598
_cell_measurement_theta_min      2.275
_cell_volume                     6286(2)
_computing_cell_refinement       'SAINT V8.32B (Bruker SAINT, 2016)'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'SAINT V8.32B (Bruker SAINT, 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      110
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73670
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         1.962
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1390 before and 0.0357 after correction. The Ratio of minimum to maximum transmission is 0.8411. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/pentane'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         14546
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+6.3211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12938
_reflns_number_total             14546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02100k2.cif
_cod_data_source_block           wcs989
_cod_depositor_comments
'Adding full bibliography for 7700273--7700274.cif.'
_cod_database_code               7700273
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.690
_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. Restrained distances
 P3-C52 \\sim P3-C52A
 with sigma of 0.01
 C54A-C52A \\sim C54-C52 \\sim C53A-C52A \\sim C53-C52
 with sigma of 0.01
 C53-C54 \\sim C53A-C54A
 with sigma of 0.01
 P2-C25 \\sim P2-C25A
 with sigma of 0.01
 C27A-C25A \\sim C27-C25 \\sim C26-C25 \\sim C26A-C25A
 with sigma of 0.01
 C26-C27 \\sim C26A-C27A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C7S \\sim C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7T \\sim
C1T \\sim C2T \\sim C3T \\sim C4T \\sim C5T \\sim C6T: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C52 \\sim C53 \\sim C54 \\sim C52A \\sim C53A \\sim C54A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C25 \\sim C26 \\sim C27 \\sim C25A \\sim C26A \\sim C27A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) = Uanis(C25A)
Uanis(C27A) = Uanis(C27)
4. Rigid body (RIGU) restrains
 C7S, C1S, C2S, C3S, C4S, C5S, C6S, C7T, C1T, C2T, C3T, C4T, C5T, C6T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C52, C53, C54, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C26, C27, C25A, C26A, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C7T)=Sof(H7TA)=Sof(H7TB)=Sof(H7TC)=Sof(C1T)=Sof(C2T)=Sof(H2T)=Sof(C3T)=
 Sof(H3T)=Sof(C4T)=Sof(H4T)=Sof(C5T)=Sof(H5T)=Sof(C6T)=Sof(H6T)=Sof(C52A)=
 Sof(H52A)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=Sof(C1S)=Sof(C2S)=
 Sof(H2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=Sof(H5S)=Sof(C6S)=
 Sof(H6S)=FVAR(1)
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(2)
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25), C28(H28), C49(H49), C52(H52), C55(H55),
 C58(H58), C52A(H52A), C25A(H25A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C33(H33), C34(H34), C35(H35),
  C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S),
  C2T(H2T), C3T(H3T), C4T(H4T), C5T(H5T), C6T(H6T)
6.c Fitted hexagon refined as free rotating group:
 C1S(C2S,C3S,C4S,C5S,C6S), C1T(C2T,C3T,C4T,C5T,C6T)
6.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C7S(H7SA,H7SB,H7SC), C7T(H7TA,H7TB,H7TC),
 C53A(H53D,H53E,H53F), C54A(H54D,H54E,H54F), C26A(H26D,H26E,H26F), C27A(H27D,
 H27E,H27F)
;
_shelx_res_checksum              72989
_olex2_submission_special_instructions 'No special instructions were received'