Linking Cr3 triangles through phosphonates and lanthanides: synthetic, structural, magnetic and EPR studies.
Zangana, Karzan H.; Pineda, Eufemio Moreno; Vitorica-Yrezabal, Iñigo J; McInnes, Eric J. L.; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 13242–13249; doi:10.1039/c4dt01264j

data_7032301
_publ_section_title
;
 Linking Cr3 triangles through phosphonates and lanthanides: synthetic,
 structural, magnetic and EPR studies.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13242
_journal_page_last               13249
_journal_paper_doi               10.1039/c4dt01264j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C92 H184 Cr6 Gd2 O44 P4, 2(C4 H9 O), H2 O, 2(O)'
_chemical_formula_sum            'C100 H204 Cr6 Gd2 O50 P4'
_chemical_formula_weight         2957.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.817(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8020(7)
_cell_length_b                   27.527(2)
_cell_length_c                   19.718(2)
_cell_measurement_reflns_used    3966
_cell_measurement_temperature    150.03(18)
_cell_measurement_theta_max      26.1460
_cell_measurement_theta_min      3.4070
_cell_volume                     7452.8(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.03(18)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   14.00   64.00   1.0000   12.6200
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000  150.0000 50

  2 omega  -12.00   93.00   1.0000   12.6200
omega____ theta____ kappa____ phi______ frames
    -       20.8673   77.0000   30.0000 105

  3 omega  -20.00   63.00   1.0000   12.6200
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000  -90.0000 83

  4 omega  -84.00   31.00   1.0000   12.6200
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -19.0000   60.0000 115
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0051689000
_diffrn_orient_matrix_UB_12      -0.0107149000
_diffrn_orient_matrix_UB_13      0.0328286000
_diffrn_orient_matrix_UB_21      -0.0050220000
_diffrn_orient_matrix_UB_22      0.0232381000
_diffrn_orient_matrix_UB_23      0.0149413000
_diffrn_orient_matrix_UB_31      -0.0511337000
_diffrn_orient_matrix_UB_32      -0.0033482000
_diffrn_orient_matrix_UB_33      -0.0018730000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2100
_diffrn_reflns_av_unetI/netI     0.2458
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.292
_refine_diff_density_min         -2.228
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         13614
_refine_ls_number_restraints     517
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1732
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6450
_reflns_number_total             13614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031805
_cod_data_source_file            c4dt01264j2.cif
_cod_data_source_block           Cr6Gd2P4
_cod_original_cell_volume        7452.9(11)
_cod_database_code               7032301
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Cr6 Gd2 O60 C100 H150 P4'
_chemical_oxdiff_usercomment     KH-50-3
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C52-C48A
 1.54 with sigma of 0.02
 C15A-C16A
 1.54 with sigma of 0.02
 C16A-C17A
 1.54 with sigma of 0.02
 C15A-C17A
 2.5 with sigma of 0.02
 C16A-C19A
 1.54 with sigma of 0.02
 C15A-C19A
 2.5 with sigma of 0.02
 C17A-C19A
 2.5 with sigma of 0.02
 O6A-C3A
 1.54 with sigma of 0.02
 C3A-C2A
 1.54 with sigma of 0.02
 C2A-C1A
 1.54 with sigma of 0.02
 C4A-C2A
 1.54 with sigma of 0.02
 C3A-C1A
 2.5 with sigma of 0.02
 C4A-C3A
 2.5 with sigma of 0.02
 C4A-C1A
 2.5 with sigma of 0.02
 C2A-O6A
 2.5 with sigma of 0.02
 O24-C57
 3 with sigma of 0.02
 C56-C57
 1.54 with sigma of 0.02
 C57-C56
 1.54 with sigma of 0.02
 C57-C58
 2.5 with sigma of 0.02
 C56-C58
 1.54 with sigma of 0.02
 C55-O24
 1.45 with sigma of 0.02
 C57-C55
 2.5 with sigma of 0.02
 C55-C56
 1.54 with sigma of 0.02
 C55-C58
 2.5 with sigma of 0.02
 C16-C17
 1.54 with sigma of 0.02
 C15-C16
 1.54 with sigma of 0.02
 C15-C17
 2.5 with sigma of 0.02
 C19-C16
 1.54 with sigma of 0.02
 C15-C19
 2.5 with sigma of 0.02
 C2-O6
 2.4 with sigma of 0.02
 C2-C4
 1.54 with sigma of 0.02
 C1-C2
 1.54 with sigma of 0.02
 C2-C3
 1.54 with sigma of 0.02
 C3-C2
 1.54 with sigma of 0.02
 C1-C2
 1.54 with sigma of 0.02
 C2-C4
 1.54 with sigma of 0.02
 C4-C1
 2.5 with sigma of 0.02
 C1-C3
 2.5 with sigma of 0.02
 C3-C4
 2.5 with sigma of 0.02
 C38-C40
 1.54 with sigma of 0.02
 C38-C41
 1.54 with sigma of 0.02
 O7-C19
 3 with sigma of 0.02
 O7-C16
 2.4 with sigma of 0.02
 C15A-O7
 1.45 with sigma of 0.02
 C61-C60
 1.54 with sigma of 0.02
 C62-C61
 2.5 with sigma of 0.02
 C60-C62
 1.6 with sigma of 0.02
 C59-C61
 2.5 with sigma of 0.02
 C59-C60
 1.54 with sigma of 0.02
 C59-C60
 1.54 with sigma of 0.02
 C59-C62
 2.5 with sigma of 0.02
 C61-O23
 3 with sigma of 0.02
 O23-C60
 2.4 with sigma of 0.02
 O23-C59
 1.42 with sigma of 0.02
 C30-C36
 1.54 with sigma of 0.02
 C35-C30A
 1.54 with sigma of 0.02
 C6-C9
 1.54 with sigma of 0.02
 C50-C52 \\sim C52-C53 \\sim C50-C53
 with sigma of 0.02
 C48A-C50 \\sim C48A-C52 \\sim C48A-C53
 with sigma of 0.02
 C33-C31 \\sim C35-C33 \\sim C31-C35
 with sigma of 0.02
 C30A-C31 \\sim C30A-C33 \\sim C30A-C35
 with sigma of 0.02
 C16-C17 \\sim C16-C15 \\sim C16-C19
 with sigma of 0.02
 C48-C54 \\sim C48-C49 \\sim C48-C51
 with sigma of 0.02
 C51-C49 \\sim C54-C49 \\sim C54-C51
 with sigma of 0.02
 C2-C1 \\sim C2-C3 \\sim C2-C4
 with sigma of 0.02
 C11-C12 \\sim C11-C14 \\sim C11-C13
 with sigma of 0.02
 C13-C12 \\sim C12-C14 \\sim C14-C13
 with sigma of 0.02
 C8-C7 \\sim C9-C8 \\sim C7-C9
 with sigma of 0.02
 C46-C45 \\sim C44-C45 \\sim C44-C46
 with sigma of 0.02
 C43-C44 \\sim C43-C45 \\sim C43-C46
 with sigma of 0.02
 O6-C3 \\sim O6A-C3A
 with sigma of 0.02
 C30-C32 \\sim C30-C34 \\sim C30-C36
 with sigma of 0.02
 C6-C7 \\sim C6-C8 \\sim C6-C9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15A \\sim C15 \\sim C16 \\sim C16A \\sim C19A \\sim C19 \\sim C17 \\sim C17A:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C4A \\sim C1 \\sim C2 \\sim C1A \\sim C3 \\sim O6 \\sim O6A \\sim C4 \\sim C3A:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1B \\sim O1C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O6A) = Uanis(O6)
Uanis(O1C) = Uanis(O23)
Uanis(O1B) = Uanis(O24)
4. Rigid body (RIGU) restrains
 C4A, C2A, C1A, C3A, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, C1, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, O6, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C15, C16, C17, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C48, C54, C51, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C48A, C47, C50, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15A, C16A, C17A, C19A, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, C59, C61, C62, O23, C55, O24, C56, C58, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C32, C34, C36, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C30A, C33, C35, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O24, C55, C57, C58, C56, O1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, O23, C59, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C30A)=1-FVAR(1)
 Sof(C30)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C48A)=1-FVAR(2)
 Sof(C48)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 Sof(H51C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16A)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(3)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(3)
 Sof(O6A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C2A)=Sof(H2A)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(4)
 Sof(O6)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(4)
 Sof(O24)=Sof(C55)=Sof(HI)=Sof(HJ)=Sof(C56)=Sof(HK)=Sof(C57)=Sof(HL)=Sof(HM)=
 Sof(HN)=Sof(C58)=Sof(HO)=Sof(HP)=Sof(HQ)=Sof(O1C)=1-FVAR(5)
 Sof(O23)=Sof(C59)=Sof(H)=Sof(HA)=Sof(C60)=Sof(HB)=Sof(C61)=Sof(HC)=Sof(HD)=
 Sof(HE)=Sof(C62)=Sof(HF)=Sof(HG)=Sof(HH)=Sof(O1B)=FVAR(5)
 Fixed Sof: O1A(0.5) H1AD(0.5) H1AE(0.5)
6.a Free rotating group:
 O1A(H1AD,H1AE)
6.b Rotating group:
 O12(H12A,H12B)
6.c Ternary CH refined with riding coordinates:
 C2(H2), C16(H16), C60(HB), C56(HK), C16A(H16A), C2A(H2A)
6.d Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C15(H15A,H15B), C59(H,HA), C55(HI,HJ), C15A(H15C,H15D), C3A(H3AA,
 H3AB)
6.e Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C12(H12C,H12D,H12E), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C61(HC,HD,HE), C62(HF,HG,HH), C57(HL,HM,HN), C58(HO,HP,HQ), C19A(H19D,
 H19E,H19F), C17A(H17D,H17E,H17F), C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              26335
_olex2_submission_special_instructions 'No special instructions were received'