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_7703905
_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 H17 O2 P'
_chemical_formula_sum            'C14 H17 O2 P'
_chemical_formula_weight         248.24
_chemical_properties_physical    Air-sensitive,Moisture-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'
_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                 93.452(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8705(3)
_cell_length_b                   9.7423(2)
_cell_length_c                   11.9176(2)
_cell_measurement_reflns_used    2898
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.4210
_cell_measurement_theta_min      4.0620
_cell_volume                     1259.83(5)
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     40.00  92.00   1.00    4.60    --   37.91 178.00 150.00   52
  2  \w     -6.00  64.00   1.00    4.60    --   37.91 -99.00-180.00   70
  3  \w     57.00 105.00   1.00    4.60    --   37.91 178.00  90.00   48
  4  \w     21.00  96.00   1.00    4.60    --   37.91  57.00 -90.00   75
  5  \w     93.00 167.00   1.00   18.40    --  107.00  61.00  60.00   74
  6  \w     42.00  69.00   1.00   18.40    --  107.00-111.00-150.00   27
  7  \w     84.00 120.00   1.00   18.40    --  107.00  77.00 150.00   36
  8  \w     38.00  79.00   1.00   18.40    --  107.00 -95.00 -60.00   41
  9  \w     55.00 123.00   1.00   18.40    --  107.00 -61.00 -60.00   68
 10  \w     51.00  78.00   1.00   18.40    --  107.00 -95.00-120.00   27
 11  \w     39.00  64.00   1.00   18.40    --  107.00 -95.00  90.00   25
 12  \w     92.00 171.00   1.00   18.40    --  107.00  45.00   0.00   79
 13  \w    150.00 175.00   1.00   18.40    --  107.00  77.00 150.00   25
 14  \w     89.00 170.00   1.00   18.40    --  107.00  77.00  30.00   81
;
_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      0.0663558000
_diffrn_orient_matrix_UB_12      -0.1392881000
_diffrn_orient_matrix_UB_13      0.0132216000
_diffrn_orient_matrix_UB_21      -0.0016084000
_diffrn_orient_matrix_UB_22      -0.0140546000
_diffrn_orient_matrix_UB_23      -0.1288788000
_diffrn_orient_matrix_UB_31      0.1255287000
_diffrn_orient_matrix_UB_32      0.0733385000
_diffrn_orient_matrix_UB_33      0.0001229000
_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  0.0194
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4524
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.722
_diffrn_reflns_theta_min         4.074
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85176
_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 colourless'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2237
_reflns_number_total             2407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00864h2.cif
_cod_data_source_block           compound-2e
_cod_depositor_comments
'Adding full bibliography for 7703903--7703909.cif.'
_cod_database_code               7703905
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C14 H17 O2 P1 '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10)
2.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C13(H13a,H13b,H13c)
;
_shelx_res_checksum              18212
_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 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.690