(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_1545532
_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         'C34 H47 N3 Na O5 P3, C36 H52 N2 Na O6 P3'
_chemical_formula_sum            'C70 H99 N5 Na2 O11 P6'
_chemical_formula_weight         1418.34
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2017-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-19 deposited with the CCDC.
2017-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.246(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6426(13)
_cell_length_b                   11.7291(6)
_cell_length_c                   24.5253(12)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      70.11
_cell_measurement_theta_min      3.29
_cell_volume                     7740.1(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_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, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Platinum135 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 0.997
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Platinum135'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  '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  0.0510
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            127799
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         70.256
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.5220
_exptl_absorpt_correction_T_min  0.4127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0720 before and 0.0595 after correction. The Ratio of minimum to maximum transmission is 0.7906. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_recrystallization_method thf
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         14712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0443P)^2^+5.6379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13096
_reflns_number_total             14712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00300e2.cif
_cod_data_source_block           gb_rj_mh5_48
_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               1545532
_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. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C6A)
3. Others
 Sof(H7BC)=Sof(H7BD)=Sof(H5BC)=Sof(H5BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(H5AA)=Sof(H5AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C65(H65), C68(H68), C56(H56), C31(H31), C19(H19), C22(H22), C53(H53), C34(H34)
4.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C3(H3A,H3B), C41(H41A,H41B), C2(H2A,H2B), C7(H7AA,H7AB),
 C7(H7BC,H7BD), C8(H8A,H8B), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6A,H6B),
 C6A(H6AA,H6AB)
4.c Aromatic/amide H refined with riding coordinates:
 C61(H61), C50(H50), C49(H49), C51(H51), C62(H62), C29(H29), C63(H63),
 C27(H27), C28(H28), C17(H17), C16(H16), C15(H15)
4.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C57(H57A,H57B,
 H57C), C69(H69A,H69B,H69C), C58(H58A,H58B,H58C), C21(H21A,H21B,H21C), C24(H24A,
 H24B,H24C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C20(H20A,H20B,H20C),
 C32(H32A,H32B,H32C), C54(H54A,H54B,H54C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C4(H4A,H4B,H4C), C42(H42A,H42B,H42C), C39(H39A,H39B,H39C), C55(H55A,
 H55B,H55C), C1(H1A,H1B,H1C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              9855
_olex2_exptl_crystal_mounting_method fomblin
_olex2_submission_special_instructions 'No special instructions were received'