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_7048719
_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         'C32 H50 Br2 Cu2 N6 O4 P4'
_chemical_formula_sum            'C32 H50 Br2 Cu2 N6 O4 P4'
_chemical_formula_weight         993.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                86.8260(14)
_cell_angle_beta                 79.3340(16)
_cell_angle_gamma                84.3383(15)
_cell_formula_units_Z            2
_cell_length_a                   9.22027(18)
_cell_length_b                   12.2451(2)
_cell_length_c                   18.8242(3)
_cell_measurement_reflns_used    23355
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.1090
_cell_measurement_theta_min      2.0150
_cell_volume                     2076.91(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  19.00   0.50   12.00    --  -20.00 -72.00-180.00  258
  2  \w   -110.00  16.00   0.50   12.00    --  -20.00   0.00  36.00  252
  3  \w    -87.00   9.00   0.50   12.00    --  -20.00 -72.00  36.00  192
  4  \w    -44.00  -1.00   0.50   12.00    --  -20.00  72.00 -36.00   86
  5  \w    -59.00 -28.50   0.50   12.00    --  -20.00  72.00-180.00   61
  6  \w   -110.00  25.00   0.50   12.00    --  -20.00   0.00 108.00  270
  7  \w   -110.00  10.00   0.50   12.00    --  -20.00 -72.00 108.00  240
  8  \w    -69.00  19.00   0.50   12.00    --  -20.00 -72.00-108.00  176
  9  \w    -42.50  -8.00   0.50   12.00    --  -20.00  72.00  36.00   69
 10  \w    -59.00 -28.50   0.50   12.00    --  -20.00  72.00-108.00   61
 11  \w    -59.00 -28.50   0.50   12.00    --  -20.00  72.00 108.00   61
 12  \w   -110.00  39.00   0.50   12.00    --  -20.00   0.00 -36.00  298
 13  \w    -78.00 -47.50   0.50   12.00    --  -20.00 -72.00 -36.00   61
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_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  0.0658
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.967
_exptl_absorpt_coefficient_mu    3.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69950
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.127
_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     465
_refine_ls_number_reflns         7296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.7255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6389
_reflns_number_total             7296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04819c2.cif
_cod_data_source_block           compound-4
_cod_original_cell_volume        2076.91(7)
_cod_database_code               7048719
_shelx_shelxl_version_number     2014/7
_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:
 C23(H23), C4(H4), C20(H20), C5(H5), C22(H22), C3(H3), C21(H21), C2(H2)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C16(H16A,H16B,
 H16C), C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C13(H13A,H13B,H13C), C32(H32A,H32B,H32C),
 C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              52770
_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
;