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_7703909
_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         '2(C16 H11 O7 P W)'
_chemical_formula_sum            'C32 H22 O14 P2 W2'
_chemical_formula_weight         1060.13
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 91.882(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0044(3)
_cell_length_b                   9.7434(3)
_cell_length_c                   32.7494(10)
_cell_measurement_reflns_used    4509
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.2370
_cell_measurement_theta_min      5.6150
_cell_volume                     3509.51(18)
_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_environment      N~2~
_diffrn_ambient_temperature      100(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.967
_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    -24.00  42.00   1.00    5.00    --    0.00 -99.00-180.00   66
  2  \w   -112.00 -18.00   1.00   30.00    --  -54.75 125.00 120.00   94
  3  \w     87.00 114.00   1.00   30.00    --   54.75 104.00 -16.00   27
  4  \w     73.00 126.00   1.00   30.00    --   54.75 125.00-120.00   53
  5  \w     35.00 110.00   1.00   30.00    --   54.75  57.00  60.00   75
  6  \w     52.00 131.00   1.00   60.00    --  109.50 -50.00  90.00   79
  7  \w     46.00 132.00   1.00   60.00    --  109.50 -64.00 -90.00   86
  8  \w     40.00  93.00   1.00   60.00    --  109.50 -50.00-150.00   53
  9  \w     95.00 172.00   1.00   60.00    --  109.50  50.00 -90.00   77
 10  \w    106.00 131.00   1.00   60.00    --  109.50 -50.00-150.00   25
 11  \w     90.00 131.00   1.00   60.00    --  109.50 -77.00   0.00   41
 12  \w     75.00 175.00   1.00   60.00    --  109.50  25.00  30.00  100
;
_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      0.1130521000
_diffrn_orient_matrix_UB_12      -0.0677978000
_diffrn_orient_matrix_UB_13      -0.0178676000
_diffrn_orient_matrix_UB_21      0.0681192000
_diffrn_orient_matrix_UB_22      0.0147360000
_diffrn_orient_matrix_UB_23      0.0415902000
_diffrn_orient_matrix_UB_31      -0.0469225000
_diffrn_orient_matrix_UB_32      -0.1420937000
_diffrn_orient_matrix_UB_33      0.0128603000
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11703
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.754
_diffrn_reflns_theta_min         5.283
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46354
_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    2.006
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.094
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6635
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0461P)^2^+46.8306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5673
_reflns_number_total             6635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00864h2.cif
_cod_data_source_block           compound-5d
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '100 (10)' was changed
to '100(10)' -- the value was reformatted.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7703903--7703909.cif.
;
_cod_database_code               7703909
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H24 O14 P2 W2'
_shelx_estimated_absorpt_t_max   0.348
_shelx_estimated_absorpt_t_min   0.175
_reflns_odcompleteness_completeness 98.94
_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
2. Restrained distances
 W2-C2AA \\sim W2-C2AB
 with sigma of 0.02
 C2AA-O5AA \\sim C2AB-O4A
 with sigma of 0.02
 W2-O5AA \\sim W2-O4A
 with sigma of 0.04
 W2-C2AA \\sim W2-C1AA
 with sigma of 0.02
 C2AA-O5AA \\sim C1AA-O0AA
 with sigma of 0.02
 W2-O5AA \\sim W2-O0AA
 with sigma of 0.04
 W2-O0AA \\sim W2-O0AB
 with sigma of 0.04
 W2-C1AA \\sim W2-C1AB
 with sigma of 0.02
 C1AA-O0AA \\sim C1AB-O0AB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5AA \\sim O2AA \\sim O4A \\sim O4B \\sim O0AB \\sim O0AC \\sim O0AA: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O0AC \\sim O0AB \\sim O4B \\sim O4A \\sim O2AA \\sim O5AA \\sim O0AA: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O2AA \\sim O4A \\sim O4B \\sim O0AB \\sim O0AC \\sim O0AA \\sim O1AA \\sim
O5AA: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
O4B \\sim O4A \\sim O2AA \\sim O1AA \\sim O5AA \\sim O0AA \\sim O0AC \\sim
O0AB: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C0 \\sim C0AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O1B \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C0AA \\sim C0: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O1A \\sim O1B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(O1AA) = Uanis(C1AA) = Uanis(C1AC) = Uanis(O0AC) =
Uanis(O0AA) = Uanis(C1AB) = Uanis(O0AB) = Uanis(C2AC) = Uanis(O4B) = Uanis(O4A)
= Uanis(C2AB) = Uanis(C2AA) = Uanis(O5AA) = Uanis(C4AA) = Uanis(O2AA)
Uanis(O1A) = Uanis(C0) = Uanis(C0AA) = Uanis(O1B)
4. Rigid body (RIGU) restrains
 C0AA, C0, C4AA, C2AB, O4A, O2AA, C2AA, O1AA, O5AA, C1A, C1AB, C2AC, O4B, O0AB,
  C1AC, O0AC, C1AA, O0AA, O1B, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(W2)=Sof(C2AA)=Sof(O5AA)=Sof(W2A)=Sof(O2AA)=Sof(C4AA)=1-FVAR(1)
 Sof(C2AB)=Sof(O4A)=Sof(C1AB)=Sof(O0AB)=Sof(C2AC)=Sof(O4B)=Sof(C1AC)=Sof(O0AC)=
 FVAR(1)
 Sof(O4AA)=1-FVAR(2)
 Sof(O3AA)=FVAR(2)
 Sof(C1A)=Sof(O1AA)=1-FVAR(3)
 Sof(C1AA)=Sof(O0AA)=FVAR(3)
 Fixed Sof: O1B(0.55) C0(0.45) C6AA(0.5) H6AA(0.5) H6AB(0.5) C5AA(0.5)
 H5AA(0.5) H5AB(0.5) C0AA(0.55) O1A(0.45)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C25(H25A,H25B), C4(H4A,H4B), C3(H3A,H3B), C7AA(H7AA,H7AB),
 C6AA(H6AA,H6AB), C5AA(H5AA,H5AB)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C8(H8), C7(H7), C9(H9), C11(H11), C19(H19), C20(H20), C10(H10),
 C22(H22), C21(H21)
;
_shelx_res_checksum              39411
_olex2_date_sample_data_collection 2019-07-09
_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 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.697