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_7703908
_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         'C15 H29 P Si2'
_chemical_formula_sum            'C15 H29 P Si2'
_chemical_formula_weight         296.53
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Pyrophoric
_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                 113.140(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2774(2)
_cell_length_b                   24.2123(3)
_cell_length_c                   13.4741(2)
_cell_measurement_reflns_used    8781
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.6330
_cell_measurement_theta_min      3.9950
_cell_volume                     3683.12(11)
_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 1.000
_diffrn_measured_fraction_theta_max 0.986
_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     31.00 104.00   1.00    1.41    --   37.66  57.00-120.00   73
  2  \w     72.00 108.00   1.00    1.41    --   37.66 178.00-180.00   36
  3  \w     80.00 107.00   1.00    1.41    --   37.66  38.00 150.00   27
  4  \w     19.00  46.00   1.00    1.41    --   37.66  38.00 150.00   27
  5  \w    -25.00  73.00   1.00    1.41    --   37.66 -99.00-180.00   98
  6  \w    -30.00  10.00   1.00    1.41    --   37.66 -77.00 120.00   40
  7  \w     86.00 161.00   1.00    5.62    --  107.00  30.00  30.00   75
  8  \w     44.00 118.00   1.00    5.62    --  107.00 -45.00 -30.00   74
  9  \w     43.00  93.00   1.00    5.62    --  107.00 -91.00   1.56   50
 10  \w     93.00 166.00   1.00    5.62    --  107.00  61.00-120.00   73
 11  \w     45.00 115.00   1.00    5.62    --  107.00 -61.00-120.00   70
 12  \w     58.00 114.00   1.00    5.62    --  107.00 -91.00  73.67   56
 13  \w     40.00 128.00   1.00    5.62    --  107.00 -30.00-150.00   88
 14  \w     86.00 142.00   1.00    5.62    --  107.00 -91.00 125.41   56
 15  \w     56.00  83.00   1.00    5.62    --  107.00 -95.00-180.00   27
 16  \w     54.00  81.00   1.00    5.62    --  107.00 -91.00 125.41   27
;
_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      0.0470171000
_diffrn_orient_matrix_UB_12      -0.0595575000
_diffrn_orient_matrix_UB_13      0.0086957000
_diffrn_orient_matrix_UB_21      0.1278353000
_diffrn_orient_matrix_UB_22      0.0215281000
_diffrn_orient_matrix_UB_23      0.0561615000
_diffrn_orient_matrix_UB_31      -0.0082456000
_diffrn_orient_matrix_UB_32      -0.0062427000
_diffrn_orient_matrix_UB_33      0.1106037000
_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  0.0212
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16420
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.627
_diffrn_reflns_theta_min         3.651
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72754
_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_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0516P)^2^+1.1425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6594
_reflns_number_total             7100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00864h2.cif
_cod_data_source_block           MesP(SiMe3)2
_cod_depositor_comments
;
Adding full bibliography for 7703903--7703909.cif.

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C15 H29 P Si2)'
_cod_original_formula_sum        'C30 H58 P2 Si4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     593.06
_cod_database_code               7703908
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H29 P1 Si2'
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.376
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C24(H24), C11(H11), C26(H26)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C), C5(H5A,H5B,
 H5C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C2(H2A,H2B,
 H2C), C20(H20A,H20B,H20C), C3(H3A,H3B,H3C), C21(H21A,H21B,H21C), C1(H1A,H1B,
 H1C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              40473
_olex2_submission_original_sample_id VS004
_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 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.656