Synthesis of 1,2,3-tripnictolide anions by reaction of group 15 Zintl ions with acetylene. Isolation of [E/3C/2H/2]^-^ (E = P, As) and preliminary reactivity studies
Robert S. P. Turbervill; Jose M. Goicoechea; Chem.Commun. 48 (2012) 6100–; doi:10.1039/c2cc32244g

data_7107853
_publ_contact_author_fax         '+44 1865 272690'
_publ_section_title
;
 Synthesis of 1,2,3-tripnictolide anions by reaction of group 15 Zintl
 ions with acetylene. Isolation of [E/3C/2H/2]^-^ (E = P, As) and
 preliminary reactivity studies
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_journal_name_full               Chem.Commun.
_journal_page_first              6100
_journal_paper_doi               10.1039/c2cc32244g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C18 H36 K N2 O6, C2 H2 As3'
_chemical_formula_sum            'C20 H38 As3 K N2 O6'
_chemical_formula_weight         666.38
_chemical_name_systematic
;
[K(2,2,2-crypt)][As3C2H2]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.6210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.00950(10)
_cell_length_b                   10.83120(10)
_cell_length_c                   25.7344(3)
_cell_measurement_reflns_used    8702
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.2479
_cell_measurement_theta_min      3.4486
_cell_volume                     2776.58(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_full        76.44
_diffrn_reflns_theta_max         76.44
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    5.944
_exptl_absorpt_correction_T_max  0.5357
_exptl_absorpt_correction_T_min  0.4142
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5759
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+2.4945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                5407
_reflns_number_total             5759
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc32244g.txt
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:
data name '_contact_author_fax' replaced with
'_publ_contact_author_fax' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7107853