Synthesis and reactivity of selenium functionalised allylidynes and propargylidynes.
Hill, Anthony F.; Manzano, Richard A.; Ward, Jas S.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14621–14629; doi:10.1039/c8dt02370k

data_7047597
_publ_section_title
;
 Synthesis and reactivity of selenium functionalised allylidynes and
 propargylidynes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14621
_journal_page_last               14629
_journal_paper_doi               10.1039/c8dt02370k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H33 B N6 O2 Se2 W'
_chemical_formula_sum            'C32 H33 B N6 O2 Se2 W'
_chemical_formula_weight         886.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-08-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.0753(2)
_cell_length_b                   20.7893(6)
_cell_length_c                   31.3879(8)
_cell_measurement_reflns_used    19552
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.9110
_cell_measurement_theta_min      1.9600
_cell_volume                     6574.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -65.00   86.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.9799   77.0000  120.0000 151

  2 omega  -27.00  124.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -       19.2924   77.0000 -120.0000 151

  3 omega  -27.00  124.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -       19.2924   77.0000    0.0000 151

  4 omega  -20.00   34.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.9799  -99.0000   60.0000 54

  5 omega -122.00  -34.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.9799  178.0000  120.0000 88

  6 omega  -27.00  124.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -       19.2924   77.0000  150.0000 151

  7 omega  -78.00   65.00   1.0000   82.5000
omega____ theta____ kappa____ phi______ frames
    -       19.2924  -57.0000  -60.0000 143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0050843000
_diffrn_orient_matrix_UB_12      0.0323678000
_diffrn_orient_matrix_UB_13      -0.0069775000
_diffrn_orient_matrix_UB_21      0.0066986000
_diffrn_orient_matrix_UB_22      0.0107389000
_diffrn_orient_matrix_UB_23      0.0213363000
_diffrn_orient_matrix_UB_31      0.0698878000
_diffrn_orient_matrix_UB_32      0.0013018000
_diffrn_orient_matrix_UB_33      -0.0025652000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1324
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            92531
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.959
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       plate
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.2089
_exptl_crystal_size_mid          0.1771
_exptl_crystal_size_min          0.0282
_refine_diff_density_max         3.787
_refine_diff_density_min         -3.072
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6714
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0941
_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^)+(0.0411P)^2^+283.4473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5525
_reflns_number_total             6714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02370k2.cif
_cod_data_source_block           RAM003_scale
_cod_depositor_comments
'Adding full bibliography for 7047597--7047599.cif.'
_cod_database_code               7047597
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.379
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N21, N22, C21, C22, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N11, N12, C11, C12, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W1, O4, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W1, O5, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N31, N32, C31, C32, C33, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C22(H22), C32(H32), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              9708
_ins_header
;
TITL RAM001_scale in Pbcm 
REM Pbcm (#57 in standard setting)
CELL 0.71073  10.075299  20.789336  31.387891  90.0000  90.0000  90.0000
ZERR    8.00   0.000179   0.000561   0.000764   0.0000   0.0000   0.0000
LATT  1
SYMM -x,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x,-y+1/2,-z 
SFAC C H B N O Se W
UNIT 256.00 264.00 8.00 48.00 16.00 16.00 8.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'