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_7107852
_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         'C12 H24 K O6, C2 H2 P3'
_chemical_formula_sum            'C14 H26 K O6 P3'
_chemical_formula_weight         422.36
_chemical_name_systematic
;
[K(18-crown-6)][P3C2H2]
;
_space_group_IT_number           11
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_symmetry_space_group_name_Hall  '-P 2yb'
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_atom_sites_solution_hydrogens   geom
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.3280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.08640(10)
_cell_length_b                   15.5733(2)
_cell_length_c                   14.6129(2)
_cell_measurement_reflns_used    6998
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0842
_cell_measurement_theta_min      3.0621
_cell_volume                     2040.46(4)
_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)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
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_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'omega scans'
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_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       11
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_exptl_absorpt_coefficient_mu    4.732
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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
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
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_refine_ls_number_reflns         4387
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_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0610P)^2^+1.4170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                4155
_reflns_number_total             4387
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc32244g.txt
_cod_data_source_block           1b
_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)/m'
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