"Low-coordinate" 1,2-oxaphosphetanes - a new opportunity in coordination and main group chemistry.
Kyri, A. W.; Gleim, F.; García Alcaraz, A; Schnakenburg, G.; Espinosa Ferao, A.; Streubel, R.; Chemical communications (Cambridge, England) 54 (2018) 7123–7126; doi:10.1039/c8cc02963f

data_7121602
_publ_section_title
;
 &quot;Low-coordinate&quot; 1,2-oxaphosphetanes - a new opportunity in
 coordination and main group chemistry.
;
_journal_issue                   52
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7123
_journal_page_last               7126
_journal_paper_doi               10.1039/c8cc02963f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C27 H21 Mo O6 P'
_chemical_formula_sum            'C27 H21 Mo O6 P'
_chemical_formula_weight         568.35
_chemical_name_systematic        AKY-623
_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     heavy
_audit_creation_date             2017-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-03-06 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                76.188(2)
_cell_angle_beta                 83.221(2)
_cell_angle_gamma                73.4935(19)
_cell_formula_units_Z            2
_cell_length_a                   9.6734(4)
_cell_length_b                   10.6787(4)
_cell_length_c                   12.9836(5)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.31
_cell_volume                     1246.92(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35439
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         3.236
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0840 before and 0.0485 after correction. The Ratio of minimum to maximum transmission is 0.8930. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+1.4712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5670
_reflns_number_total             6000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02963f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7121602--7121604.cif.'
_cod_database_code               7121602
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C1S)=Sof(H1S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=Sof(H2BC)=Sof(H2BD)=
 1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              30496
_olex2_submission_special_instructions 'No special instructions were received'