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_7037472
_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 H48 Cd3 N24 O30 P6, C H4 O'
_chemical_formula_sum            'C61 H52 Cd3 N24 O31 P6'
_chemical_formula_weight         2140.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-19
_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                90
_cell_angle_beta                 97.434(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.112(6)
_cell_length_b                   16.605(5)
_cell_length_c                   19.463(4)
_cell_measurement_reflns_used    5698
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.99
_cell_measurement_theta_min      2.20
_cell_volume                     8048(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0843
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53635
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.044
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.572229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0549 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.5722.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       block
_exptl_crystal_F_000             4272
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform, methanol mixture'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         15764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0754P)^2^+3.4849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11079
_reflns_number_total             15764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03537f2.cif
_cod_data_source_block           1420484
_cod_depositor_comments
'Adding full bibliography for 7037469--7037472.cif.'
_cod_database_code               7037472
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C54(H54), C45(H45), C12(H12), C15(H15), C49(H49), C3(H3), C24(H24),
 C4(H4), C53(H53), C32(H32), C37(H37), C25(H25), C52(H52), C2(H2), C40(H40),
 C5(H5), C55(H55), C22(H22), C17(H17), C50(H50), C43(H43), C47(H47), C9(H9),
 C23(H23), C8(H8), C10(H10), C38(H38), C27(H27), C48(H48), C14(H14), C13(H13),
 C44(H44), C30(H30), C39(H39), C7(H7), C33(H33), C038(H038), C039(H039),
 C29(H29), C03B(H03B), C35(H35), C34(H34), C03E(H03E), C18(H18), C20(H20),
 C19(H19), C28(H28)
2.b Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C)
2.c Idealised tetrahedral OH refined as rotating group:
 O31(H31)
;
_shelx_res_checksum              83581
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'