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_7037470
_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 Cu N20 O24 P6 Zn2, 4(N O3), 4(H2 O), 2.92(O), C2 H3 N'
_chemical_formula_sum            'C62 H71 Cu N25 O42.92 P6 Zn2'
_chemical_formula_weight         2233.17
_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             2015-11-05
_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                70.090(6)
_cell_angle_beta                 84.713(6)
_cell_angle_gamma                80.116(6)
_cell_formula_units_Z            1
_cell_length_a                   11.827(4)
_cell_length_b                   12.597(4)
_cell_length_c                   16.144(6)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.27
_cell_volume                     2226.4(13)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_laue_measured_fraction_full 0.977
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11282
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         3.979
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.658003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.1114 before and 0.0317 after correction. The Ratio of minimum to maximum transmission is 0.6580. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile, methanol'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         7641
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1502P)^2^+3.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5601
_reflns_number_total             7641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03537f2.cif
_cod_data_source_block           1420483
_cod_depositor_comments
'Adding full bibliography for 7037469--7037472.cif.'
_cod_database_code               7037470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H9A,H9B} of O9
 At 1.5 times of:
  All C(H,H,H) groups, {H1AA,H1AB} of O1A, {H7AA,H7AB} of O7AA, {H1FA,H1FB}
  of O1F, {H7A,H7B} of O7, {H8A,H8B} of O8
2. Restrained distances
 N11-O15 = N11-O14 = N11-O13
 1.22 with sigma of 0.02
 N12A-O16A = N12A-O18A = N12A-O17A
 1.2 with sigma of 0.02
 C1B-C6AA
 1.5 with sigma of 0.02
 N0AA-C1B
 1.2 with sigma of 0.02
 C1B-C6AA
 1.54 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.002
Uanis(N11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(O17A) \\sim Ueq, Uanis(O18A) \\sim Ueq, Uanis(O16A) \\sim Ueq,
Uanis(N12A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(O1F) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C1B) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(N12B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(O16B) \\sim Ueq, Uanis(O17B) \\sim Ueq, Uanis(O18B) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.002
Uanis(O16C) \\sim Ueq, Uanis(O17C) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.002
Uanis(C6AA) \\sim Ueq, Uanis(O7AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(N0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O16D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O14, O13, O15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O18B)=Sof(O16B)=Sof(O17B)=Sof(N12B)=Sof(O17C)=Sof(O16C)=1-FVAR(1)
 Sof(O16A)=Sof(O18A)=Sof(N12A)=Sof(O17A)=Sof(O16D)=FVAR(1)
 Sof(O7AA)=Sof(H7AA)=Sof(H7AB)=1-FVAR(2)
 Sof(O1A)=Sof(H1AA)=Sof(H1AB)=FVAR(2)
 Fixed Sof: C6AA(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C1B(0.5) N0AA(0.5)
6.a Riding coordinates:
 O1A(H1AA,H1AB), O7AA(H7AA,H7AB)
6.b Free rotating group:
 O1F(H1FA,H1FB)
6.c Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B)
6.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C4(H4), C6(H6), C18(H18), C2(H2), C8(H8), C11(H11),
 C12(H12), C14(H14), C15(H15), C17(H17), C19(H19), C1A(H1A), C0AA(H0AA),
 C1C(H1C), C1D(H1D), C1E(H1E), C1G(H1G), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25)
6.e Idealised Me refined as rotating group:
 C6AA(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              20182
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'