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_7037469
_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 H64 N22 O31.4 P6 Zn3, 4(H2 O), 2(N O3), 0.6(O), 2(C H4 O)'
_chemical_formula_sum            'C62 H80 N24 O44 P6 Zn3'
_chemical_formula_weight         2247.43
_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
_audit_creation_date             2015-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-24 deposited with the CCDC.
2015-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                101.701(5)
_cell_angle_beta                 90.287(6)
_cell_angle_gamma                100.396(6)
_cell_formula_units_Z            1
_cell_length_a                   11.434(4)
_cell_length_b                   12.410(4)
_cell_length_c                   15.945(5)
_cell_measurement_reflns_used    3241
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.25
_cell_volume                     2177.1(12)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Brucker 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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14452
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         4.109
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.532583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0666 before and 0.0323 after correction.
The Ratio of minimum to maximum transmission is 0.5326.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.591
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.161
_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     625
_refine_ls_number_reflns         7523
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1550P)^2^+6.2736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2265
_refine_ls_wR_factor_ref         0.2502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5821
_reflns_number_total             7523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03537f2.cif
_cod_data_source_block           1420482
_cod_depositor_comments
'Adding full bibliography for 7037469--7037472.cif.'
_cod_database_code               7037469
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N11-O19 = N11-O17 = N11-O18
 1.22 with sigma of 0.02
 N11-O18 = N11-O19 = N11-O17
 1.22 with sigma of 0.02
 N11-O18 = N11-O19 = N11-O17
 1.22 with sigma of 0.02
 N11-O18 = N11-O19 = N11-O17
 1.22 with sigma of 0.02
 O1AA-C1B
 1.42 with sigma of 0.002
 O17-O18
 2.2 with sigma of 0.04
 O17-O19
 2.2 with sigma of 0.04
 O18-O19
 2.2 with sigma of 0.04
 O18-O19
 2.2 with sigma of 0.04
 O18-O19
 2.2 with sigma of 0.04
 O18-O19
 2.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N12) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(N12)
\\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.002
Uanis(O0AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(O1AA) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: O10(0.7) O8(0.7) O0AA(0.3) O1A(0.3)
 Fixed Uiso: O18(0.30237) O19(0.30482) N11(0.28146) O17(0.30187)
5.a Riding coordinates:
 O13(H13A,H13B), O12(H12A,H12B), O7(H7A,H7B), O20(H20A,H20B), O22(H22A,H22B)
5.b Rotating group:
 O11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30)
5.d Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC)
5.e Idealised tetrahedral OH refined as rotating group:
 O1AA(H1AA)
;
_shelx_res_checksum              98491
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'