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_7048715
_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 Cu2 I2 N6 O4 P4'
_chemical_formula_sum            'C32 H50 Cu2 I2 N6 O4 P4'
_chemical_formula_weight         1087.54
_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                88.319(2)
_cell_angle_beta                 82.651(3)
_cell_angle_gamma                84.948(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2630(3)
_cell_length_b                   12.1825(3)
_cell_length_c                   18.6917(7)
_cell_measurement_reflns_used    6773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      3.0
_cell_volume                     2083.49(12)
_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      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0373
_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       -11
_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            32062
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.678
_exptl_absorpt_coefficient_mu    2.698
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.306
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS RIGAKU 1999'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.146
_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     465
_refine_ls_number_reflns         7309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0309P)^2^+3.3227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6485
_reflns_number_total             7309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04819c2.cif
_cod_data_source_block           compound-5
_cod_database_code               7048715
_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), C20(H20), C6(H6), C21(H21), C22(H22), C3(H3), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C26(H26A,H26B,H26C), C12(H12A,H12B,
 H12C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C28(H28A,
 H28B,H28C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              39484
_olex2_submission_special_instructions 'No special instructions were received'