Cyclo-oligomerization of isocyanates with Na(PH2) or Na(OCP) as “P−” anion sources
Heift, Dominikus; Benkő, Zoltán; Grützmacher, Hansjörg; Jupp, Andrew R.; Goicoechea, Jose M.; Chem. Sci. 6 (2015) 4017–; doi:10.1039/C5SC00963D

data_1519644
_publ_section_title
;
 Cyclo-oligomerization of isocyanates with Na(PH2) or Na(OCP) as
 &#x201C;P&#x2212;&#x201D; anion sources
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4017
_journal_paper_doi               10.1039/C5SC00963D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C12 H24 K O6, C52 H80 N4 O4 P'
_chemical_formula_sum            'C64 H92 K N4 O10 P'
_chemical_formula_weight         1147.48
_chemical_name_systematic
;
 [K(18-crown-6)][P{(CO)2[N(Dipp)]2}2]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.271(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2330(3)
_cell_length_b                   19.9093(4)
_cell_length_c                   13.5733(3)
_cell_measurement_reflns_used    6922
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.8623
_cell_measurement_theta_min      3.5980
_cell_volume                     3233.79(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19203
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.045
_diffrn_reflns_theta_min         3.601
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98061
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pyridine, ether'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.306(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11186
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.6914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                9838
_reflns_number_total             11186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00963d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:
'__exptl_absorpt_process_details' tag replaced with
'_exptl_absorpt_process_details' tag.

Automatic conversion script
Id: cif_correct_tags 3376 2015-05-07 07:48:27Z andrius 

 Adding full bibliography for 1519640--1519644.cif.
;
_cod_original_cell_volume        3233.79(14)
_cod_database_code               1519644
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2014-3
_shelx_res_checksum              36177