Catechol and 1,2,4,5-tetrahydroxybenzene functionalized cyclodiphosphazane ligands: synthesis, structural studies, and transition metal complexesɸ
Pandey, Madhusudan K.; Kunchur, Harish S.; Ananthnag, GS; Mague, Joel T.; Balakrishna, Maravanji Shivaramaiah; Dalton Transactions  (2019) –; doi:10.1039/C8DT04819C

data_7048720
_publ_section_title
;
 Catechol and 1,2,4,5-tetrahydroxybenzene functionalized
 cyclodiphosphazane ligands: synthesis, structural studies, and transition
 metal complexes&#x0278;
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04819C
_journal_year                    2019
_chemical_formula_moiety         'C34 H58 Cl4 N4 O4 P4 Pd4'
_chemical_formula_sum            'C34 H58 Cl4 N4 O4 P4 Pd4'
_chemical_formula_weight         1278.12
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-05 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.152(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.4158(13)
_cell_length_b                   10.4693(7)
_cell_length_c                   17.2657(16)
_cell_measurement_reflns_used    6011
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.2100
_cell_measurement_theta_min      2.2840
_cell_volume                     2785.7(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -110.00  70.00   0.50   16.00    --  -20.00   0.00-108.00  360
  2  \w    -70.00   5.00   0.50   16.00    --  -20.00 -72.00  36.00  150
  3  \w    -79.00   5.00   0.50   16.00    --  -20.00 -72.00-108.00  168
  4  \w    -58.50  -6.00   0.50   16.00    --  -20.00  72.00-180.00  105
  5  \w    -59.00 -47.00   0.50   16.00    --  -20.00  72.00  36.00   24
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku saturn 724+'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20568
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.352
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50596
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       needle
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.409
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0757P)^2^+13.1932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3398
_reflns_number_total             4889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04819c2.cif
_cod_data_source_block           compound-15
_cod_database_code               7048720
_shelx_shelxl_version_number     2014/7
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C16) = Uanis(C17)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C),
 C10(H10A,H10B,H10C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              73742
_shelx_fab_checksum              60571
_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
- Detector area scaling
;