(Phosphanyl)phosphaketenes as building blocks for novel phosphorus heterocycles
Hansmann, Max M.; Ruiz, David A.; Liu, Liu (Leo); Jazzar, Rodolphe; Bertrand, Guy; Chem. Sci. 8 (2017) 3720–; doi:10.1039/C7SC00300E

data_1545527
_publ_section_title
;
 (Phosphanyl)phosphaketenes as building blocks for novel phosphorus
 heterocycles
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3720
_journal_paper_doi               10.1039/C7SC00300E
_journal_volume                  8
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H58 N2 Na O7 P3'
_chemical_formula_sum            'C40 H58 N2 Na O7 P3'
_chemical_formula_weight         794.78
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.09 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-19 deposited with the CCDC.
2017-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7779(4)
_cell_length_b                   14.7189(4)
_cell_length_c                   21.2291(6)
_cell_measurement_reflns_used    9263
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.86
_cell_measurement_theta_min      3.65
_cell_volume                     4305.2(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77347
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         70.008
_diffrn_reflns_theta_min         3.654
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0879 before and 0.0729 after correction.
The Ratio of minimum to maximum transmission is 0.8467.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method THF
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 3287 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8126
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0622
_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^)+(0.1022P)^2^+3.7244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                7785
_reflns_number_total             8126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00300e2.cif
_cod_data_source_block           gb_liuamidep4_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1545527--1545532.cif.
;
_cod_database_code               1545527
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C27B)
Uanis(C26A) = Uanis(C26B)
Uanis(P2) = Uanis(P2A)
Uanis(P3) = Uanis(P3A)
Uanis(C11A) = Uanis(C11)
Uanis(C12) = Uanis(C12A)
3. Rigid body (RIGU) restrains
 O5, C36, C35, C34, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C27B)=Sof(H27A)=
 Sof(H27B)=Sof(H0AC)=Sof(H0AD)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C26A)=Sof(H26C)=
 Sof(H26D)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
 Sof(P2A)=Sof(P3A)=1-FVAR(2)
 Sof(P2)=Sof(P3)=FVAR(2)
 Sof(H10A)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C10(H10A), C7(H7), C19(H19), C22(H22)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C32(H32A,H32B), C25(H25C,H25D), C25(H25A,H25B), C31(H31A,
 H31B), C30(H30A,H30B), C36(H36A,H36B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C26B(H26A,H26B), C27B(H27A,H27B), C27A(H27C,H27D), C26A(H26C,
 H26D), C0AA(H0AC,H0AD), C0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4), C15(H15), C17(H17), C16(H16)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C20(H20A,H20B,
 H20C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              79018
_olex2_exptl_crystal_mounting_method fomblin
_olex2_submission_special_instructions 'No special instructions were received'