Studies on the reactivity of group 15 Zintl ions with carbodiimides: synthesis and characterization of a heptaphosphaguanidine dianion
Robert S. P. Turbervill; Jose M. Goicoechea; Chem.Commun. 48 (2012) 1470–; doi:10.1039/c1cc12089a

data_7107257
_publ_contact_author_fax         '+44 1865 272690'
_publ_section_title
;
 Studies on the reactivity of group 15 Zintl ions with carbodiimides:
 synthesis and characterization of a heptaphosphaguanidine dianion
;
_journal_name_full               Chem.Commun.
_journal_page_first              1470
_journal_paper_doi               10.1039/c1cc12089a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         '2(C12 H24 K O6), C25 H35 N2 P7'
_chemical_formula_sum            'C49 H83 K2 N2 O12 P7'
_chemical_formula_weight         1187.16
_chemical_name_common            (K-(18-crown-6))2(H(P7C(NDipp)2))
_chemical_name_systematic
;
[K-(18-crown-6)]2{H[P7C(NDipp)2]}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.2460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   14.14770(10)
_cell_length_b                   19.1536(2)
_cell_length_c                   69.3584(8)
_cell_measurement_reflns_used    79224
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.4937
_cell_measurement_theta_min      3.1227
_cell_volume                     18780.3(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar 7 2011,18:06:32)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar 7 2011,18:06:32)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar 7 2011,18:06:32)
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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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  area
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            168980
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         66.50
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_T_max  0.7684
_exptl_absorpt_correction_T_min  0.4025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar 7 2011,18:06:32)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7560
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2392
_refine_ls_number_reflns         33114
_refine_ls_number_restraints     1139
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+44.3741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                30883
_reflns_number_total             33114
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1cc12089a.txt
_cod_data_source_block           1
_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      P2(1)/c
_cod_database_code               7107257