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_7048718
_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         'C28 H44 Br4 Cu4 N4 O4 P4'
_chemical_formula_sum            'C28 H44 Br4 Cu4 N4 O4 P4'
_chemical_formula_weight         1198.35
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.0690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3981(9)
_cell_length_b                   16.3342(10)
_cell_length_c                   17.8607(11)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      29.3667
_cell_measurement_theta_min      2.2359
_cell_volume                     4133.0(4)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2014)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2014)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2014)'
_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      150.15
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58368
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    6.089
_exptl_absorpt_correction_T_max  0.47
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0361P)^2^+11.7319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6369
_reflns_number_total             7277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04819c2.cif
_cod_data_source_block           compound-7
_cod_database_code               7048718
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.470
_shelx_estimated_absorpt_t_min   0.312
_exptl_absorpt_special_details   'fine-focus sealed tube'
_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:
 C3(H3), C4(H4), C5(H5), C6(H6), C28(H28), C27(H27), C26(H26), C25(H25)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              87798
_olex2_submission_special_instructions 'No special instructions were received'