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_1519641
_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         'C20 H36 N4 O4 P, Na, C4 H8 O'
_chemical_formula_sum            'C24 H44 N4 Na O5 P'
_chemical_formula_weight         522.59
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-02-14 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.339(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3693(13)
_cell_length_b                   14.6742(10)
_cell_length_c                   21.9183(17)
_cell_measurement_reflns_used    8325
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.35
_cell_volume                     5802.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CMOS 100-Bruker Area Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81997
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2008/1 Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic blocks'
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         8325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+5.9821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                6162
_reflns_number_total             8325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc00963d2.cif
_cod_data_source_block
spiro-bi-pentacyclo-(p(co)(nbu)(co)(nbu))-_na(dme)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1519640--1519644.cif.

2023-04-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H88 N8 Na2 O10 P2'
_cod_original_formula_weight         1045.18
_cod_original_formula_moiety         'C48 H88 N8 Na2 O10 P2'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1519641