Phosphacycloalkyldiones: synthesis and coordinative behaviour of 6- and 7-member cyclic diketophosphanyls.
Pearce, Kyle G.; Simenok, Vladimir; Crossley, Ian R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5482–5492; doi:10.1039/d0dt00864h

data_7703907
_publ_section_title
;
 Phosphacycloalkyldiones: synthesis and coordinative behaviour of 6- and
 7-member cyclic diketophosphanyls.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5482
_journal_page_last               5492
_journal_paper_doi               10.1039/d0dt00864h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C14 H15 O7 P W'
_chemical_formula_sum            'C14 H15 O7 P W'
_chemical_formula_weight         510.08
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-09
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3442(2)
_cell_length_b                   12.5495(2)
_cell_length_c                   21.9424(4)
_cell_measurement_reflns_used    3379
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.5830
_cell_measurement_theta_min      5.4160
_cell_volume                     3399.17(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  12.00   1.00   27.63    --   37.66   0.00-180.00   32
  2  \w     -2.00  54.00   1.00   27.63    --   37.66 -57.00 -30.00   56
  3  \w     24.00 105.00   1.00   27.63    --   37.66   0.00-180.00   81
  4  \w     90.00 172.00   1.00  110.53    --  107.00  61.00-120.00   82
  5  \w    126.00 158.00   1.00  110.53    --  107.00  61.00 -60.00   32
  6  \w     55.00  82.00   1.00  110.53    --  107.00 -95.00  30.00   27
  7  \w     93.00 177.00   1.00  110.53    --  107.00 111.00  90.00   84
  8  \w     57.00 102.00   1.00  110.53    --  107.00 -61.00-180.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0537620000
_diffrn_orient_matrix_UB_12      -0.0361715000
_diffrn_orient_matrix_UB_13      -0.0598303000
_diffrn_orient_matrix_UB_21      0.1114892000
_diffrn_orient_matrix_UB_22      0.0009412000
_diffrn_orient_matrix_UB_23      0.0316320000
_diffrn_orient_matrix_UB_31      -0.0159638000
_diffrn_orient_matrix_UB_32      -0.1173102000
_diffrn_orient_matrix_UB_33      0.0186760000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6770
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.718
_diffrn_reflns_theta_min         4.029
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0495P)^2^+3.2855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2866
_reflns_number_total             3219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00864h2.cif
_cod_data_source_block           compound-5c
_cod_depositor_comments
'Adding full bibliography for 7703903--7703909.cif.'
_cod_database_code               7703907
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C14 H15 P W O7 '
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              51690
_olex2_date_sample_data_collection 2019-02-18
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.737
_oxdiff_exptl_absorpt_empirical_full_min 0.733