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_7047598
_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_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C52 H54 B2 N12 O4 Se2 W2, C6 H6'
_chemical_formula_sum            'C58 H60 B2 N12 O4 Se2 W2'
_chemical_formula_weight         1536.43
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-07-15
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2018-08-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.1006(17)
_cell_angle_beta                 81.6539(15)
_cell_angle_gamma                84.5006(14)
_cell_formula_units_Z            2
_cell_length_a                   10.1236(2)
_cell_length_b                   15.4789(3)
_cell_length_c                   19.9039(4)
_cell_measurement_reflns_used    17740
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     2989.55(11)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36975
_diffrn_reflns_theta_full        72.281
_diffrn_reflns_theta_max         72.281
_diffrn_reflns_theta_min         3.298
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.846
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/hexane'
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.039
_refine_diff_density_max         2.68
_refine_diff_density_min         -1.03
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9384
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         11721
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.0015490
_refine_ls_shift/su_mean         0.0000248
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.190E+04 0.316E+04 0.199E+04 867. 213. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0979
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0978
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10564
_reflns_number_total             11767
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.20
_oxford_diffrn_Wilson_scale      0.23
_oxford_refine_ls_r_factor_ref   0.0411
_oxford_refine_ls_scale          2.280(9)
_oxford_reflns_number_all        11722
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Jas\Desktop\RAM012(F6)( At 23:28 on'
_cod_data_source_file            c8dt02370k2.cif
_cod_data_source_block           RAM012(F6)(6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047597--7047599.cif.
;
_cod_original_cell_volume        2989.55(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7047598
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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