Hydrophosphination-type reactivity promoted by bismuth phosphanides: scope and limitations.
Schwamm, R. J.; Fulton, J. R.; Coles, M. P.; Fitchett, C. M.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2068–2071; doi:10.1039/c7dt00226b

data_7041870
_publ_section_title
;
 Hydrophosphination-type reactivity promoted by bismuth phosphanides:
 scope and limitations.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2068
_journal_page_last               2071
_journal_paper_doi               10.1039/c7dt00226b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C47 H73 Bi N3 O2 P Si2'
_chemical_formula_sum            'C47 H73 Bi N3 O2 P Si2'
_chemical_formula_weight         1008.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-12 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                87.6009(17)
_cell_angle_beta                 78.6468(18)
_cell_angle_gamma                66.154(2)
_cell_formula_units_Z            6
_cell_length_a                   17.6927(4)
_cell_length_b                   18.2618(4)
_cell_length_c                   25.0124(5)
_cell_measurement_reflns_used    36031
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      32.7300
_cell_measurement_theta_min      3.0230
_cell_volume                     7240.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -38.00  -12.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5680   57.0000  -60.0000 26

  2 omega  -37.00  -11.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5680   19.0000  -90.0000 26

  3 omega   -9.00   22.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6305   77.0000    0.0000 31

  4 omega  -11.00   89.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6305   77.0000 -150.0000 100

  5 omega   -1.00   86.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6305   57.0000   90.0000 87

  6 omega   62.00   87.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6305   37.0000  120.0000 25

  7 omega  -54.00   37.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       17.6305  -37.0000  -60.0000 91

  8 omega -103.00  -78.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5680  178.0000    0.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0444028000
_diffrn_orient_matrix_UB_12      -0.0126808000
_diffrn_orient_matrix_UB_13      -0.0066429000
_diffrn_orient_matrix_UB_21      -0.0043458000
_diffrn_orient_matrix_UB_22      0.0273166000
_diffrn_orient_matrix_UB_23      -0.0213587000
_diffrn_orient_matrix_UB_31      -0.0028791000
_diffrn_orient_matrix_UB_32      0.0299908000
_diffrn_orient_matrix_UB_33      0.0183765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62744
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.645
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         3.362
_refine_diff_density_min         -2.155
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1546
_refine_ls_number_reflns         26168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+10.5113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22715
_reflns_number_total             26168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00226b2.cif
_cod_data_source_block           Compound-6-55mc44
_cod_depositor_comments
;
Adding full bibliography for 7041870--7041871.cif.

2017-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C141 H219 Bi3 N9 O6 P3 Si6'
_cod_original_formula_weight         3024.63
_cod_original_formula_moiety         '3(C47 H73 Bi N3 O2 P Si2)'
_cod_original_formula_units_Z            2
_cod_database_code               7041870
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C23(H23), C26(H26), C36(H36), C42(H42), C101(H101),
 C104(H104), C117(H117), C120(H120), C130(H130), C136(H136), C54(H54), C57(H57),
  C70(H70), C73(H73), C83(H83), C89(H89)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
 C47(H47A,H47B), C131(H13D,H13E), C132(H13F,H13G), C133(H13H,H13I), C134(H13J,
 H13K), C135(H13L,H13M), C137(H13N,H13O), C138(H13P,H13Q), C139(H13R,H13S),
 C140(H14D,H14E), C141(H14F,H14G), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,
 H86B), C87(H87A,H87B), C88(H88A,H88B), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B)
2.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C108(H10P,H10Q,H10R), C61(H61A,H61B,H61C)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C19(H19), C20(H20), C21(H21), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C97(H97), C98(H98), C99(H99), C113(H113),
 C114(H114), C115(H115), C124(H124), C125(H125), C126(H126), C127(H127),
 C128(H128), C50(H50), C51(H51), C52(H52), C67(H67), C68(H68), C69(H69),
 C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
2.e Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C105(H10G,H10H,H10I), C106(H10J,
 H10K,H10L), C107(H10M,H10N,H10O), C109(H10S,H10T,H10U), C110(H11D,H11E,H11F),
 C118(H11G,H11H,H11I), C119(H11J,H11K,H11L), C121(H12D,H12E,H12F), C122(H12G,
 H12H,H12I), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,
 H75B,H75C)
;
_olex2_submission_special_instructions 'No special instructions were received'