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_7039952
_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_absolute_configuration syn
_chemical_formula_moiety
'C30 H28 Gd N6 Ni O21 P6, Cl, H Na O0.5, 2.5(H2 O), 3(O)'
_chemical_formula_sum            'C30 H34 Cl Gd N6 Na Ni O27 P6'
_chemical_formula_weight         1370.85
_chemical_name_systematic        Compound-4
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 106.794(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6611(11)
_cell_length_b                   16.9747(8)
_cell_length_c                   15.2845(7)
_cell_measurement_reflns_used    7418
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      21.553
_cell_measurement_theta_min      2.239
_cell_volume                     5628.7(5)
_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 0.999
_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  0.0983
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59575
_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         27.850
_diffrn_reflns_theta_min         1.523
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.811
_exptl_absorpt_correction_T_max  0.8992
_exptl_absorpt_correction_T_min  0.7379
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details
;
 Flack x determined using 2749 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         13356
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0973P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8222
_reflns_number_total             13356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02023b2.cif
_cod_data_source_block           Compound-4
_cod_depositor_comments
'Adding full bibliography for 7039946--7039953.cif.'
_cod_database_code               7039952
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.713
_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(O10A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O4A) \\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 0.01
Uanis(Cl1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5A) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O17A) \\sim Ueq, Uanis(P6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(O17) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(P4A)=Sof(O11A)=Sof(H11B)=Sof(O10A)=1-FVAR(1)
 Sof(P4)=Sof(O10)=Sof(O11)=Sof(H11)=FVAR(1)
 Sof(O4)=Sof(P2A)=Sof(O5A)=Sof(H5A)=Sof(O6A)=1-FVAR(2)
 Sof(P2)=Sof(O5)=Sof(O6)=Sof(H2)=Sof(O4A)=FVAR(2)
 Sof(P6A)=Sof(O17A)=Sof(O18A)=Sof(H18B)=1-FVAR(3)
 Sof(P6)=Sof(O17)=Sof(O18)=Sof(H18)=FVAR(3)
 Fixed Sof: O22(0.5) H22A(0.5) H22B(0.5) O27(0.25) H27A(0.25) H27B(0.25)
 O35(0.75) H35A(0.75) H35B(0.75) O30(0.5) O33(0.5) O34(0.5) H34A(0.5) H34B(0.5)
 O36(0.5) H36A(0.5) H36B(0.5) O31(0.5) H31A(0.5) H31B(0.5) O28(0.5) O29(0.5)
4.a Riding coordinates:
 O20(H20A,H20B), O21(H21A,H21B), O27(H27A,H27B), O11A(H11B), O35(H35A,H35B),
 O34(H34A,H34B), O36(H36A,H36B), O31(H31A,H31B), O18A(H18B)
4.b Rotating group:
 O22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11A), C13(H13A),
 C14(H14), C17(H17), C18(H18A), C20(H20), C21(H21), C23(H23), C24(H24),
 C27(H27), C28(H28), C30(H30)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O6(H2), O9(H9), O11(H11), O13(H13), O18(H18), O5A(H5A)
;
_shelx_res_checksum              18746
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'