[3+2]-Annulation of platinum-bound azomethine ylides with distal C[double bond, length as m-dash]C bonds of N-allenamides.
Chakrabarty, Indradweep; Inamdar, Suleman M.; Akram, Manjur O.; Gade, Amol B.; Banerjee, Subhrashis; Bera, Saibal; Patil, Nitin T.; Chemical communications (Cambridge, England) 53 (2016) 196–199; doi:10.1039/c6cc07874e

data_7119612
_publ_section_title
;
 [3+2]-Annulation of platinum-bound azomethine ylides with distal C[double
 bond, length as m-dash]C bonds of N-allenamides.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              196
_journal_page_last               199
_journal_paper_doi               10.1039/c6cc07874e
_journal_volume                  53
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         '(C38 H32 N2 O2 S)'
_chemical_formula_sum            'C38 H32 N2 O2 S'
_chemical_formula_weight         580.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-22
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:34:12, GUI svn.r4372)
;
_audit_update_record
;
2016-08-23 deposited with the CCDC.
2016-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   5.8561(3)
_cell_length_b                   23.2600(9)
_cell_length_c                   44.864(2)
_cell_measurement_reflns_used    3187
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      52.6010
_cell_measurement_theta_min      4.2800
_cell_volume                     6111.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.8745
_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     28.00 126.00   1.00   28.13    --   54.00  37.00   0.00   98
  2  \w    100.00 144.00   1.00   28.13    --  108.00 111.00 -30.00   44
  3  \w    104.00 133.00   1.00   28.13    --  108.00 111.00-120.00   29
  4  \w    120.00 172.00   1.00   28.13    --  108.00  37.00  60.00   52
  5  \w     49.00  87.00   1.00   28.13    --  108.00-111.00-150.00   38
  6  \w     36.00 108.00   1.00   28.13    --  108.00-111.00-180.00   72
  7  \w     39.00 134.00   1.00   28.13    --  108.00 -37.00-120.00   95
  8  \w     31.00  95.00   1.00   28.13    --   54.00-125.00  90.00   64
  9  \w     25.00  55.00   1.00   28.13    --   54.00-125.00 -60.00   30
 10  \w    -39.00  17.00   1.00   28.13    --    0.00 -37.00 120.00   56
 11  \w     11.00  37.00   1.00   28.13    --    0.00  77.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0715797000
_diffrn_orient_matrix_UB_12      -0.0221975000
_diffrn_orient_matrix_UB_13      0.0309617000
_diffrn_orient_matrix_UB_21      -0.1388284000
_diffrn_orient_matrix_UB_22      0.0484985000
_diffrn_orient_matrix_UB_23      0.0148190000
_diffrn_orient_matrix_UB_31      -0.2116359000
_diffrn_orient_matrix_UB_32      -0.0392867000
_diffrn_orient_matrix_UB_33      0.0007709000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            16067
_diffrn_reflns_theta_full        70.8981
_diffrn_reflns_theta_max         70.90
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.2624
_exptl_crystal_description       needle
_exptl_crystal_F_000             2448.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2337
_refine_diff_density_min         -0.3382
_refine_diff_density_rms         0.0554
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.78(2)
_refine_ls_d_res_high            0.8158
_refine_ls_d_res_low             12.5791
_refine_ls_goodness_of_fit_ref   1.0560
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    118
_refine_ls_number_parameters     778
_refine_ls_number_reflns         10301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0560
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.0718
_refine_ls_shift/su_mean         0.0018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.1283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0.739
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              28
_reflns_limit_k_min              -28
_reflns_limit_l_max              54
_reflns_limit_l_min              -53
_reflns_number_gt                6783
_reflns_number_total             11780
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc07874e2.cif
_cod_data_source_block           INDRA2
_cod_original_cell_volume        6111.0(5)
_cod_database_code               7119612
_chemical_oxdiff_formula         'C10 H10 N10 O10 S10'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H1g of C1g, H19 of C19, H72 of C72, H71 of C71, H12 of C12, H58 of C58, H38
  of C38, H59 of C59, {H17a,H17b} of C17, H32 of C32, H46 of C46, H79 of C79,
  H78 of C78, H54 of C54, H31 of C31, H55 of C55, H37 of C37, H6 of C6, H26 of
  C26, H3 of C3, H4 of C4, {H52a,H52b} of C52, H11 of C11, H74 of C74, H5 of C5,
   H48 of C48, H81 of C81, H15 of C15, H40 of C40, H82 of C82, H21 of C21, H14
  of C14, H25 of C25, H75 of C75, H41 of C41, H23 of C23, H66 of C66, H24 of
  C24, H47 of C47, H64 of C64, H22 of C22, H45 of C45, H60 of C60, {H83a,H83b,
  H83c} of C83, H8 of C8, H1a of C1a, H1b of C1b, H1c of C1c, H1d of C1d, H1e
  of C1e, H1f of C1f
 At 1.5 times of:
  {H16a,H16b,H16c} of C16, {H76a,H76b,H76c} of C76, {H42a,H42b,H42c} of C42
2.a Ternary CH refined with riding coordinates:
 C54(H54), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C52(H52a,H52b), C17(H17a,H17b)
2.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C55(H55), C37(H37), C6(H6), C26(H26), C3(H3), C4(H4), C11(H11),
 C74(H74), C5(H5), C48(H48), C81(H81), C15(H15), C40(H40), C72(H72), C71(H71),
 C12(H12), C58(H58), C38(H38), C59(H59), C32(H32), C46(H46), C79(H79), C78(H78),
  C82(H82), C21(H21), C14(H14), C25(H25), C75(H75), C41(H41), C23(H23),
 C66(H66), C24(H24), C47(H47), C64(H64), C22(H22), C45(H45), C60(H60), C8(H8),
 C1a(H1a), C1b(H1b), C1c(H1c), C1d(H1d), C1e(H1e), C1f(H1f), C1g(H1g)
2.d Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C76(H76a,H76b,H76c), C42(H42a,H42b,H42c), C83(H83a,H83b,
 H83c)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.648