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_7039949
_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 H28 Co Gd N6 O20 P6, 6.25(H2 O), 0.25(O)'
_chemical_formula_sum            'C30 H40.5 Co Gd N6 O26.5 P6'
_chemical_formula_weight         1311.18
_chemical_name_systematic        Compound-3a
_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                 116.436(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.1648(18)
_cell_length_b                   17.1628(12)
_cell_length_c                   23.0284(18)
_cell_measurement_reflns_used    6060
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.848
_cell_measurement_theta_min      2.571
_cell_volume                     8905.9(11)
_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 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_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  0.0604
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29738
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.946
_diffrn_reflns_theta_min         1.491
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  1.0204
_exptl_absorpt_correction_T_min  0.8405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_description       needle
_exptl_crystal_F_000             5244
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         10663
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7646
_reflns_number_total             10663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02023b2.cif
_cod_data_source_block           Compound-3a
_cod_depositor_comments
'Adding full bibliography for 7039946--7039953.cif.'
_cod_original_formula_sum        'C30 H40.50 Co Gd N6 O26.50 P6'
_cod_database_code               7039949
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.405
_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(P1X) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4X) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.005
Uanis(O4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O27A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2X) \\sim Ueq, Uanis(O3X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
3. Others
 Sof(P2)=Sof(O4)=Sof(H4)=1-FVAR(1)
 Sof(P1X)=Sof(O4A)=Sof(H4AA)=FVAR(1)
 Sof(O16)=Sof(O18)=Sof(O17)=Sof(H17)=1-FVAR(2)
 Sof(O2X)=Sof(H2X)=Sof(O4X)=Sof(O3X)=FVAR(2)
 Sof(O19A)=Sof(H19C)=Sof(H19D)=Sof(O20A)=Sof(H20C)=Sof(H20D)=1-FVAR(3)
 Sof(O19)=Sof(H19A)=Sof(H19B)=Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(3)
 Fixed Sof: H26A(0.5) H26B(0.5) O28(0.25) H28A(0.25) H28B(0.25) O29(0.25)
 O27(0.5) H27A(0.5) H27B(0.5) H25A(0.5) H25B(0.5) O27A(0.5) H27C(0.5) H27D(0.5)
4.a Riding coordinates:
 O3(H3), O26(H26A,H26B), O28(H28A,H28B), O22(H22A,H22B), O21(H21A,H21B),
 O23(H23A,H23B), O27(H27A,H27B), O25(H25A,H25B), O4A(H4AA), O27A(H27C,H27D),
 O19A(H19C,H19D)
4.b Free rotating group:
 O24(H24A,H24B)
4.c Rotating group:
 O19(H19A,H19B), O20(H20A,H20B), O20A(H20C,H20D)
4.d Aromatic/amide H refined with riding coordinates:
 C11(H11A), C1(H1), C14(H14), C21(H21), C17(H17A), C24(H24), C10(H10),
 C30(H30), C13(H13A), C27(H27), C3(H3A), C4(H4A), C28(H28), C8(H8), C7(H7),
 C23(H23), C18(H18), C20(H20)
4.e Idealised tetrahedral OH refined as rotating group:
 O11(H11), O13(H13), O17(H17), O2X(H2X), O9(H9), O4(H4)
;
_shelx_res_checksum              73269
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'