Molecular, 1D and 2D assemblies from hexakis(3-pyridyloxy)cyclophosphazene containing 20-membered metallamacrocyclic motifs.
Suriya Narayanan, Ramakirushnan; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2273–2283; doi:10.1039/c5dt03537f

data_7037471
_publ_section_title
;
 Molecular, 1D and 2D assemblies from
 hexakis(3-pyridyloxy)cyclophosphazene containing 20-membered
 metallamacrocyclic motifs.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2273
_journal_page_last               2283
_journal_paper_doi               10.1039/c5dt03537f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C60 H60 Cd2 N20 O24 P6, 9(H2 O), 2(N O3)'
_chemical_formula_sum            'C60 H78 Cd2 N22 O39 P6'
_chemical_formula_weight         2142.06
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-24 deposited with the CCDC.
2015-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.615(5)
_cell_angle_beta                 93.250(5)
_cell_angle_gamma                106.564(5)
_cell_formula_units_Z            1
_cell_length_a                   11.634(5)
_cell_length_b                   12.742(5)
_cell_length_c                   16.197(5)
_cell_measurement_reflns_used    2812
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.18
_cell_measurement_theta_min      2.34
_cell_volume                     2269.8(15)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       "'Bruker SMART"
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12201
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.094
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.475245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0726 before and 0.0297 after correction.
The Ratio of minimum to maximum transmission is 0.4752.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       plate
_exptl_crystal_F_000             1090
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Aqueous Ethanol'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.163
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8290
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0910
_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^)+(0.1902P)^2^+4.8166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2616
_refine_ls_wR_factor_ref         0.2920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6031
_reflns_number_total             8290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03537f2.cif
_cod_data_source_block           1420485
_cod_depositor_comments
'Adding full bibliography for 7037469--7037472.cif.'
_cod_database_code               7037471
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N11-O24 = N11-O25 = N11-O26
 1.22 with sigma of 0.02
 N11-O24 = N11-O25 = N11-O26
 1.22 with sigma of 0.02
 O25-O26
 2.1 with sigma of 0.04
 O24-O26
 2.1 with sigma of 0.04
 O24-O25
 2.1 with sigma of 0.04
 O24-O25
 2.1 with sigma of 0.04
 O24-O25
 2.1 with sigma of 0.04
 O26-O25
 2.1 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O21) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O16)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O23) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N9)
\\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.002
Uanis(O16) = Uanis(O18) = Uanis(O19) = Uanis(O22) = Uanis(O21) = Uanis(O20) =
Uanis(O23) = Uanis(O17)
4. Rigid body (RIGU) restrains
 O25, O24, N11, O26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O16(0.5) H16A(0.5) H16B(0.5) O23(0.5) H23A(0.5) H23B(0.5) O18(0.5)
 H18A(0.5) H18B(0.5) O19(0.5) H19A(0.5) H19B(0.5) O22(0.5) H22A(0.5) H22B(0.5)
 O21(0.5) H21A(0.5) H21B(0.5) O20(0.5) H20A(0.5) H20B(0.5)
 Fixed Uiso: O24(0.2) N11(0.21464) O25(0.26293) O26(0.21343)
6.a Riding coordinates:
 O17(H17A,H17B), O16(H16A,H16B), O23(H23A,H23B), O18(H18A,H18B), O19(H19A,
 H19B), O22(H22A,H22B), O21(H21A,H21B), O20(H20A,H20B)
6.b Rotating group:
 O10(H10A,H10B), O12(H12A,H12B), O11(H11A,H11B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C23(H23), C5(H5), C9(H9), C2(H2), C17(H17), C3(H3), C10(H10),
 C22(H22), C20(H20), C8(H8), C12(H12), C25(H25), C24(H24), C15(H15), C13(H13),
 C18(H18), C27(H27), C19(H19), C28(H28), C14(H14), C29(H29), C30(H30)
;
_shelx_res_checksum              89363
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'