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_7703906
_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         'C17 H26 Cl2 O2 P2 Pt'
_chemical_formula_sum            'C17 H26 Cl2 O2 P2 Pt'
_chemical_formula_weight         590.31
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            4
_cell_length_a                   7.4569(9)
_cell_length_b                   10.591(2)
_cell_length_c                   26.251(4)
_cell_measurement_reflns_used    1197
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.9010
_cell_measurement_theta_min      3.3560
_cell_volume                     2073.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_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    -36.00  31.00   1.00   47.50    --    5.00  18.00  58.00   67
  2  \w   -125.00 -97.00   1.00   47.50    --  -89.00  18.00  58.00   28
  3  \w     48.00  91.00   1.00   47.50    --    5.00  18.00  58.00   43
  4  \w   -175.00  -2.00   1.00   47.50    --  -89.00  60.00-180.00  173
  5  \w   -161.00  -4.00   1.00   47.50    --  -89.00  60.00 120.00  157
  6  \w   -108.00  -1.00   1.00   47.50    --  -89.00  57.00 150.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0551756000
_diffrn_orient_matrix_UB_12      0.0537849000
_diffrn_orient_matrix_UB_13      -0.0522670000
_diffrn_orient_matrix_UB_21      -0.0315175000
_diffrn_orient_matrix_UB_22      -0.1303474000
_diffrn_orient_matrix_UB_23      -0.0244795000
_diffrn_orient_matrix_UB_31      -0.1964664000
_diffrn_orient_matrix_UB_32      0.0358806000
_diffrn_orient_matrix_UB_33      -0.0107005000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1356
_diffrn_reflns_av_unetI/netI     0.1724
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8810
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
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    1.891
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.261
_refine_diff_density_min         -3.047
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details
;
 Flack x determined using 359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3724
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.1055
_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^)+(0.1272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.3003
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                1793
_reflns_number_total             3724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00864h2.cif
_cod_data_source_block           compound-4
_cod_depositor_comments
'Adding full bibliography for 7703903--7703909.cif.'
_cod_database_code               7703906
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 H10 Cl2 O2 P2 Pt1 '
_reflns_odcompleteness_completeness 99.54
_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. Uiso/Uaniso restraints and constraints
C1 \\sim O1 \\sim C5 \\sim O2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C2 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C12 \\sim C16 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C17 \\sim C13 \\sim C15: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C2) = Uanis(C4)
Uanis(C16) = Uanis(C17) = Uanis(C14) = Uanis(C15) = Uanis(C12) = Uanis(C13)
3. Rigid body (RIGU) restrains
 C6, C11, C10, C9, C8, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C16(H16A,H16B), C3(H3A,H3B), C12(H12A,H12B), C14(H14A,H14B),
 C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
4.c Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C10,C11)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              73346
_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 2.350
_oxdiff_exptl_absorpt_empirical_full_min 0.272