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_7039948
_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 H40 Gd2 N6 O24 P6, 0.5(O2), 12(H2 O), 4(Cl), 0.5(H2 O2)'
_chemical_formula_sum            'C30 H65 Cl4 Gd2 N6 O38 P6'
_chemical_formula_weight         1760.00
_chemical_name_systematic        Compound-2
_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
_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                104.138(7)
_cell_angle_beta                 100.605(7)
_cell_angle_gamma                98.755(7)
_cell_formula_units_Z            1
_cell_length_a                   10.362(3)
_cell_length_b                   10.819(3)
_cell_length_c                   14.686(4)
_cell_measurement_reflns_used    4532
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.226
_cell_measurement_theta_min      2.537
_cell_volume                     1535.3(7)
_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      296.15
_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 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0852
_diffrn_reflns_av_unetI/netI     0.1134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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            18987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.955
_diffrn_reflns_theta_min         1.984
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.573
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1081 before and 0.0802 after correction.
The Ratio of minimum to maximum transmission is 0.6056.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       needle
_exptl_crystal_F_000             877
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.855
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0752P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5311
_reflns_number_total             7328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02023b2.cif
_cod_data_source_block           Compound-2
_cod_depositor_comments
'Adding full bibliography for 7039946--7039953.cif.'
_cod_original_cell_volume        1535.5(7)
_cod_database_code               7039948
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.303
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O19B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
3. Others
 Sof(O19B)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(O19A)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O20B)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(O20A)=Sof(H20A)=Sof(H20B)=FVAR(2)
 Fixed Sof: O18(0.5) H17(0.5)
4.a Riding coordinates:
 O3(H3), O5(H5), O7(H7), O10(H10A,H10B), O13(H13A), O20A(H20A,H20B), O19A(H19A,
 H19B), O19B(H19C,H19D), O20B(H20C,H20D)
4.b Free rotating group:
 O12(H12A,H12B), O16(H16A,H16B), O14(H14A,H14B), O15(H15A,H15B)
4.c Rotating group:
 O11(H11A,H11B), O17(H17)
4.d Aromatic/amide H refined with riding coordinates:
 N3(H3A), C11(H11), C13(H13), C14(H14), C0AA(H0AA), C1(H1A), C4(H4), C7(H7A),
 C8(H8), C10(H10)
4.e Fitted hexagon refined as free rotating group:
 N3(C11,C12,C13,C14,C15)
;
_shelx_res_checksum              91969
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'