(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_1545529
_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         'C27 H41 B N2 O P2'
_chemical_formula_sum            'C27 H41 B N2 O P2'
_chemical_formula_weight         482.37
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-16
_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                   12.9335(12)
_cell_length_b                   20.8660(18)
_cell_length_c                   10.2861(9)
_cell_measurement_reflns_used    9059
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      4.24
_cell_volume                     2775.9(4)
_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  'XL (Sheldrick, 2008)'
_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 0.999
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Pt-135'
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.328
_diffrn_reflns_theta_min         4.237
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0840 before and 0.0557 after correction. The Ratio of minimum to maximum transmission is 0.8575. 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    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_recrystallization_method toluene
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2624
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0986P)^2^+3.1945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2367
_reflns_number_total             2624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00300e2.cif
_cod_data_source_block           gb_drppcobh3
_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               1545529
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1B = B1-H1A
 1.2 with sigma of 0.02
 P2-P1 \\sim P2A-P1A
 with sigma of 0.02
 O1A-C1A \\sim O1-C1
 with sigma of 0.02
 P2A-C1A \\sim P2-C1
 with sigma of 0.02
 P1-B1 \\sim P1A-B1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(P2A) = Uanis(P2)
Uanis(P1) = Uanis(P1A)
Uanis(B1) = Uanis(B1A)
Uanis(C1A) = Uanis(C1)
Uanis(O1A) = Uanis(O1)
4. Rigid body (RIGU) restrains
 P2A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2, C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P2A)=Sof(C1A)=Sof(O1A)=Sof(P1A)=Sof(B1A)=0.5*(1-FVAR(2))
 Sof(P1)=Sof(B1)=Sof(P2)=Sof(C1)=Sof(O1)=0.5*FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C10(H10A,H10B,
 H10C)
;
_shelx_res_checksum              80135
_olex2_exptl_crystal_mounting_method fomblin
_olex2_submission_special_instructions 'No special instructions were received'