Functionalized phosphonates as building units for multi-dimensional homo- and heterometallic 3d-4f inorganic-organic hybrid-materials.
Köhler, C; Rentschler, E.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12854–12861; doi:10.1039/c6dt02023b

data_7039951
_publ_section_title
;
 Functionalized phosphonates as building units for multi-dimensional homo-
 and heterometallic 3d-4f inorganic-organic hybrid-materials.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12854
_journal_page_last               12861
_journal_paper_doi               10.1039/c6dt02023b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C30 H26 Co N6 O20 P6 Tb, 5.5(H2 O), 0.5(O)'
_chemical_formula_sum            'C30 H37 Co N6 O26 P6 Tb'
_chemical_formula_weight         1301.32
_chemical_name_systematic        Compound-3c
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.064(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.203(2)
_cell_length_b                   17.0993(14)
_cell_length_c                   22.983(2)
_cell_measurement_reflns_used    2635
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      23.340
_cell_measurement_theta_min      2.579
_cell_volume                     8897.3(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25646
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.955
_diffrn_reflns_theta_min         1.973
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.266
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0629 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.8869.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       needle
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10680
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0889P)^2^+75.5867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7015
_reflns_number_total             10680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02023b2.cif
_cod_data_source_block           Compound-3c
_cod_depositor_comments
'Adding full bibliography for 7039946--7039953.cif.'
_cod_original_cell_volume        8897.4(13)
_cod_database_code               7039951
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.612
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O18A) \\sim Ueq, Uanis(O16A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(N1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.003
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O24A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Sof(O28A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(O28)=Sof(H28A)=Sof(H28B)=FVAR(1)
 Sof(O18A)=Sof(O16A)=Sof(O17A)=Sof(H17A)=1-FVAR(2)
 Sof(O16)=Sof(H16)=Sof(O17)=Sof(O18)=FVAR(2)
 Fixed Sof: O24(0.5) H24A(0.5) H24B(0.5) H23A(0.5) H23B(0.5) O27(0.25)
 H27A(0.25) H27B(0.25) O26(0.5) O24A(0.25) H24C(0.25) H24D(0.25)
4.a Riding coordinates:
 O24(H24A,H24B), O23(H23A,H23B), O27(H27A,H27B), O21(H21A,H21B), O24A(H24C,
 H24D), O28A(H28C,H28D), O17A(H17A)
4.b Free rotating group:
 O22(H22A,H22B), O28(H28A,H28B), O25(H25A,H25B)
4.c Rotating group:
 O19(H19A,H19B), O20(H20A,H20B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C27(H27),
  C28(H28), C30(H30)
4.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O8(H8A), O13(H13A), O16(H16)
;
_shelx_res_checksum              65916
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'