(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_1545530
_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_formula_moiety         'C218 H276 N4 Na2 O6 P6'
_chemical_formula_sum            'C218 H276 N4 Na2 O6 P6'
_chemical_formula_weight         3280.21
_chemical_name_systematic        10_polym
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                85.401(7)
_cell_angle_beta                 81.374(6)
_cell_angle_gamma                78.671(5)
_cell_formula_units_Z            1
_cell_length_a                   14.6157(11)
_cell_length_b                   18.3339(15)
_cell_length_c                   23.554(2)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.13
_cell_measurement_theta_min      3.11
_cell_volume                     6110.2(9)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (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 0.986
_diffrn_measured_fraction_theta_max 0.966
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            102657
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.825
_diffrn_reflns_theta_min         1.900
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.3201
_exptl_absorpt_correction_T_min  0.1870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1094 before and 0.0825 after correction. The Ratio of minimum to maximum transmission is 0.5842. 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    0.891
_exptl_crystal_description       needle
_exptl_crystal_F_000             1772
_exptl_crystal_recrystallization_method benzene
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1157
_refine_ls_number_reflns         21898
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+14.6923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.2404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17130
_reflns_number_total             21898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00300e2.cif
_cod_data_source_block           p-1_a_sq
_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               1545530
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 C109-C108 = C110-C109 = C111-C110 = C109-C114 = C114-C111
 1.5 with sigma of 0.02
 C103-C102 = C107-C106 = C102-C101 = C106-C105 = C105-C104 = C101-C100
 1.5 with sigma of 0.02
 C107-C104
 2.13 with sigma of 0.02
 C103-C100
 2.13 with sigma of 0.02
 C111-C108
 2.13 with sigma of 0.02
 C114-O2
 2.33 with sigma of 0.02
 O3A-C107 \\sim O3-C103 \\sim O3-C100 \\sim O3A-C104 \\sim O2A-C111 \\sim
O2A-C108
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O3A)
Uanis(C103) = Uanis(C107)
Uanis(C102) = Uanis(C106)
Uanis(C101) = Uanis(C105)
Uanis(C100) = Uanis(C104)
Uanis(C114) = Uanis(C110)
Uanis(O2A) = Uanis(O2)
4. Others
 Sof(Na1A)=1-FVAR(1)
 Sof(Na1)=FVAR(1)
 Sof(O2A)=Sof(O3A)=1-FVAR(2)
 Sof(O2)=Sof(O3)=FVAR(2)
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C16B)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(H17C)=1-FVAR(3)
 Sof(C18)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(3)
 Sof(C107)=Sof(H10E)=Sof(H10F)=Sof(C105)=Sof(H10K)=Sof(H10L)=Sof(C106)=
 Sof(H10M)=Sof(H10N)=Sof(C104)=Sof(H10O)=Sof(H10P)=1-FVAR(4)
 Sof(C100)=Sof(H10Q)=Sof(H10R)=Sof(C101)=Sof(H10S)=Sof(H10T)=Sof(C102)=
 Sof(H10U)=Sof(H10V)=Sof(C103)=Sof(H10W)=Sof(H10X)=FVAR(4)
 Sof(H11C)=Sof(H11D)=Sof(H10C)=Sof(H10D)=Sof(H10I)=Sof(H10J)=Sof(C110)=
 Sof(H11E)=Sof(H11F)=1-FVAR(5)
 Sof(H11A)=Sof(H11B)=Sof(H10A)=Sof(H10B)=Sof(H10G)=Sof(H10H)=Sof(C114)=
 Sof(H11G)=Sof(H11H)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C29(H29), C80(H80)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C50(H50A,H50B), C111(H11A,H11B), C111(H11C,H11D), C109(H10C,
 H10D), C109(H10A,H10B), C107(H10E,H10F), C108(H10G,H10H), C108(H10I,H10J),
 C110(H11E,H11F), C105(H10K,H10L), C106(H10M,H10N), C104(H10O,H10P), C100(H10Q,
 H10R), C101(H10S,H10T), C102(H10U,H10V), C103(H10W,H10X), C114(H11G,H11H)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C92(H92), C14(H14), C42(H42), C93(H93), C54(H54), C56(H56), C82(H82),
 C24(H24), C75(H75), C5(H5), C61(H61), C41(H41), C86(H86), C31(H31), C11(H11),
 C20(H20), C71(H71), C10(H10), C21(H21), C96(H96), C83(H83), C95(H95), C85(H85),
  C23(H23), C45(H45), C32(H32), C13(H13), C64(H64), C34(H34), C72(H72),
 C65(H65), C44(H44), C62(H62), C74(H74), C35(H35)
5.d Idealised Me refined as rotating group:
 C99(H99A,H99B,H99C), C58(H58A,H58B,H58C), C7(H7A,H7B,H7C), C79(H79A,H79B,
 H79C), C38(H38A,H38B,H38C), C6AA(H6AA,H6AB,H6AC), C49(H49A,H49B,H49C),
 C48(H48A,H48B,H48C), C88(H88A,H88B,H88C), C78(H78A,H78B,H78C), C98(H98A,H98B,
 H98C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C), C77(H77A,H77B,H77C), C89(H89A,
 H89B,H89C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C68(H68A,H68B,H68C),
 C90(H90A,H90B,H90C), C39(H39A,H39B,H39C), C28(H28A,H28B,H28C), C69(H69A,H69B,
 H69C), C67(H67A,H67B,H67C), C18B(H18A,H18B,H18C), C16B(H16A,H16B,H16C),
 C17B(H17A,H17B,H17C), C18(H18D,H18E,H18F), C17(H17D,H17E,H17F), C16(H16D,H16E,
 H16F)
;
_shelx_res_checksum              33624
_shelx_fab_checksum              1852
_olex2_exptl_crystal_mounting_method fomblin
_olex2_submission_original_sample_id 10_polym
_olex2_submission_special_instructions 'No special instructions were received'