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_7047599
_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         'C42 H50 B2 N12 O4 Se2 W2'
_chemical_formula_sum            'C42 H50 B2 N12 O4 Se2 W2'
_chemical_formula_weight         1334.18
_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             2014-08-28
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2018-08-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                100.513(5)
_cell_angle_beta                 104.632(6)
_cell_angle_gamma                102.645(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6869(7)
_cell_length_b                   13.9225(7)
_cell_length_c                   19.4076(16)
_cell_measurement_reflns_used    2283
_cell_measurement_temperature    150
_cell_measurement_theta_max      70
_cell_measurement_theta_min      4
_cell_volume                     2885.2(4)
_computing_cell_refinement       'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_data_collection       'SuperNova, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis PRO, (Agilent Technologies, 2013)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.957
_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  0.059
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16759
_diffrn_reflns_theta_full        56.342
_diffrn_reflns_theta_max         72.234
_diffrn_reflns_theta_min         3.362
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.066
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/hexane'
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.025
_platon_squeeze_details
;
;
_refine_diff_density_max         2.21
_refine_diff_density_min         -1.64
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0015
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10898
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.0002414
_refine_ls_shift/su_mean         0.0000149
_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: 
 0.276E+04 0.426E+04 0.247E+04 950. 204. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2218
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2218
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6490
_reflns_number_total             10931
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.00
_oxford_diffrn_Wilson_scale      0.37
_oxford_refine_ls_r_factor_ref   0.1265
_oxford_refine_ls_scale          2.33(2)
_oxford_reflns_number_all        10898
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Hill Group\Desktop\Jas At 11: 9 on '
_cod_data_source_file            c8dt02370k2.cif
_cod_data_source_block           RAM010(F8)(2)
_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.
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_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7047599
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DIST 1.2, 0.03 = C(8) TO O(8) 
DIST 1.93, 0.02 = W(1) TO C(8) 
REM 
U(IJ) 0.0, 0.02 = C(8) TO O(8) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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