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_7032304
_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
'C90 H186 Cr6 Ho2 N2 O42 P4, 2(H2 O), 2.01(C4 H9 O)'
_chemical_formula_sum            'C98 H210 Cr6 Ho2 N2 O46 P4'
_chemical_formula_weight         2918.41
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2014-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                100.079(3)
_cell_angle_beta                 100.637(3)
_cell_angle_gamma                108.254(3)
_cell_formula_units_Z            1
_cell_length_a                   13.7501(4)
_cell_length_b                   14.0220(5)
_cell_length_c                   23.1827(8)
_cell_measurement_reflns_used    16145
_cell_measurement_temperature    150.04(13)
_cell_measurement_theta_max      29.2950
_cell_measurement_theta_min      3.2360
_cell_volume                     4040.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      150.04(13)
_diffrn_detector_area_resol_mean 10.3705
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_details
;
  1 omega  -15.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555  -99.0000    0.0000 37

  2 omega  -59.00   35.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555  -57.0000   90.0000 94

  3 omega  -17.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555  -99.0000    0.0000 70

  4 omega   35.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555  178.0000   90.0000 33

  5 omega  -18.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555   57.0000 -120.0000 99
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0120467000
_diffrn_orient_matrix_UB_12      0.0018961000
_diffrn_orient_matrix_UB_13      0.0285456000
_diffrn_orient_matrix_UB_21      0.0544859000
_diffrn_orient_matrix_UB_22      0.0265106000
_diffrn_orient_matrix_UB_23      0.0147861000
_diffrn_orient_matrix_UB_31      -0.0066035000
_diffrn_orient_matrix_UB_32      0.0481556000
_diffrn_orient_matrix_UB_33      -0.0001055000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38485
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.717
_diffrn_reflns_theta_min         2.826
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.200
_exptl_crystal_description       cube
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.087
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         19167
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0969P)^2^+14.0871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15129
_reflns_number_total             19167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031808
_cod_data_source_file            c4dt01264j2.cif
_cod_data_source_block           Cr6Ho2P4
_cod_original_cell_volume        4040.0(2)
_cod_database_code               7032304
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         Cr6Ho2P4C100O50H300N4
_chemical_oxdiff_usercomment     KH-56-6
_reflns_odcompleteness_completeness 99.52
_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, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C8A-C34T
 1.54 with sigma of 0.02
 C33T-C8A
 1.54 with sigma of 0.02
 C33T-C34T
 2.5 with sigma of 0.02
 O3S-H3S
 0.87 with sigma of 0.01
 C9-C2
 1.54 with sigma of 0.02
 C2-C10
 1.54 with sigma of 0.02
 C2-C1
 1.54 with sigma of 0.02
 C9-C1
 2.5 with sigma of 0.02
 C9-C10
 2.5 with sigma of 0.02
 C10-C1
 2.5 with sigma of 0.02
 C9-O4
 1.45 with sigma of 0.02
 C2-O4
 2.4 with sigma of 0.02
 C22T-C23T
 1.54 with sigma of 0.02
 C25T-C23T
 1.54 with sigma of 0.02
 C25T-C22T
 2.5 with sigma of 0.02
 C23T-C24T
 1.54 with sigma of 0.02
 C22T-C24T
 2.5 with sigma of 0.02
 C24T-C25T
 2.5 with sigma of 0.02
 O21T-C22T
 1.45 with sigma of 0.02
 C23T-O21T
 2.4 with sigma of 0.02
 C42T-C43T
 1.54 with sigma of 0.02
 C45T-C43T
 1.54 with sigma of 0.02
 C42T-C45T
 2.5 with sigma of 0.02
 C44T-C43T
 1.54 with sigma of 0.02
 C45T-C44T
 2.5 with sigma of 0.02
 C44T-C42T
 2.5 with sigma of 0.02
 O41T-C42T
 1.45 with sigma of 0.02
 C43T-O41T
 2.4 with sigma of 0.02
 C34S-C33S
 2.5 with sigma of 0.02
 C32S-C33S
 1.54 with sigma of 0.02
 C32S-C34S
 1.54 with sigma of 0.02
 N31T-C8A
 1.45 with sigma of 0.02
 N31S-C32S
 1.45 with sigma of 0.02
 C34S-N31S
 2.44 with sigma of 0.02
 C44-C43
 1.54 with sigma of 0.02
 C43-C44A
 1.54 with sigma of 0.02
 C4S-H3S
 1.920909 with sigma of 0.02
 Cr1-H3S
 2.700384 with sigma of 0.02
 C14-C15 \\sim C14-C16 \\sim C14-C17
 with sigma of 0.02
 C14A-C15A \\sim C14A-C16A \\sim C14A-C17A
 with sigma of 0.02
 C54A-C55A \\sim C54A-C56A \\sim C54A-C57A
 with sigma of 0.02
 C54-C55 \\sim C54-C56 \\sim C54-C57
 with sigma of 0.02
 C57-C55 \\sim C55-C56 \\sim C56-C57
 with sigma of 0.02
 C44-C45 \\sim C44-C46 \\sim C44-C47
 with sigma of 0.02
 C44A-C45A \\sim C44A-C46A \\sim C44A-C47A
 with sigma of 0.02
 C4A-C5A \\sim C4A-C6A \\sim C4A-C7A
 with sigma of 0.02
 C4-C5 \\sim C4-C6 \\sim C4-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C57A \\sim C57 \\sim C56A \\sim C56 \\sim C55A \\sim C55: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C33T \\sim C8A \\sim C34T \\sim C33S \\sim C32S \\sim C34S \\sim N31T \\sim
N31S: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2) = Uanis(C9)
Uanis(O2S) = Uanis(O41T) = Uanis(O4) = Uanis(O21T)
Uanis(N31S) = Uanis(N31T)
4. Rigid body (RIGU) restrains
 C15, C14, C16, C17, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14A, C15A, C16A, C17A, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, C57, C56, C54, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C1, C2, C9, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23T, C22T, O21T, C25T, C24T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42T, O41T, C43T, C44T, C45T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8A, C33T, C34T, N31T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34T, C8A, C33T, N31T, C32S, C34S, C33S, N31S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44A, C47A, C46A, C45A, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7A, C4A, C5A, C6A, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(O41T)+Sof(C43T)+Sof(H43T)+Sof(C42T)+Sof(H42A)+Sof(H42B)+Sof(C45T)+
 Sof(H45G)+Sof(H45H)+Sof(H45I)+Sof(C44T)+Sof(H44A)+Sof(H44B)+Sof(H44C)]+1*
 [Sof(C22T)+Sof(H22A)+Sof(H22B)+Sof(O21T)+Sof(C23T)+Sof(H23T)+Sof(C25T)+
 Sof(H25D)+Sof(H25E)+Sof(H25F)+Sof(C24T)+Sof(H24A)+Sof(H24B)+Sof(H24C)]+1*
 [Sof(O4)+Sof(C2)+Sof(H2)+Sof(C1)+Sof(H1A)+Sof(H1B)+Sof(H1C)+Sof(C9)+Sof(H9A)+
 Sof(H9B)+Sof(C10)+Sof(H10A)+Sof(H10B)+Sof(H10C)]=1 with esd of 0.001
 Sof(C33T)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C8A)=Sof(H8A)=Sof(C34T)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(N31T)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(N31S)=Sof(H31A)=Sof(H31B)=Sof(C33S)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34S)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C32S)=Sof(H32S)=FVAR(1)
 Sof(C14A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(2)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C54A)=Sof(C57A)=Sof(H57D)=
 Sof(H57E)=Sof(H57F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=1-FVAR(3)
 Sof(C54)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=
 Sof(H56C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(3)
 Sof(O41T)=Sof(C43T)=Sof(H43T)=Sof(C42T)=Sof(H42A)=Sof(H42B)=Sof(C45T)=
 Sof(H45G)=Sof(H45H)=Sof(H45I)=Sof(C44T)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(4)
 Sof(C22T)=Sof(H22A)=Sof(H22B)=Sof(O21T)=Sof(C23T)=Sof(H23T)=Sof(C25T)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C24T)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(5)
 Sof(O4)=Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(6)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C44A)=Sof(C46A)=Sof(H46D)=
 Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=1-FVAR(7)
 Sof(C44)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(7)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C4A)=1-FVAR(8)
 Sof(C4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(8)
6.a Free rotating group:
 O2S(H2SA,H2SB)
6.b Rotating group:
 O1S(H1SA,H1SB)
6.c Ternary CH refined with riding coordinates:
 C5S(H5S), C32S(H32S), C8A(H8A), C43T(H43T), C23T(H23T), C2(H2)
6.d Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), N31S(H31A,H31B), N31T(H31C,H31D), C42T(H42A,H42B), C22T(H22A,
 H22B), C9(H9A,H9B)
6.e Me refined with riding coordinates:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C65(H65A,H65B,H65C), C77(H77A,H77B,
 H77C), C76(H76A,H76B,H76C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C75(H75A,
 H75B,H75C), C26(H26A,H26B,H26C), C47(H47A,H47B,H47C), C5(H5A,H5B,H5C),
 C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C6S(H6SA,H6SB,H6SC), C25(H25A,H25B,
 H25C), C45(H45A,H45B,H45C), C55(H55A,H55B,H55C), C7(H7A,H7B,H7C), C56(H56A,
 H56B,H56C), C46(H46A,H46B,H46C), C6(H6A,H6B,H6C), C36(H36A,H36B,H36C),
 C7S(H7SA,H7SB,H7SC), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C33S(H33A,H33B,
 H33C), C34S(H34A,H34B,H34C), C57(H57A,H57B,H57C), C33T(H33D,H33E,H33F),
 C34T(H34D,H34E,H34F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C15A(H15D,
 H15E,H15F), C56A(H56D,H56E,H56F), C57A(H57D,H57E,H57F), C55A(H55D,H55E,H55F),
 C45T(H45G,H45H,H45I), C44T(H44A,H44B,H44C), C25T(H25D,H25E,H25F), C24T(H24A,
 H24B,H24C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C45A(H45D,H45E,H45F),
 C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              26005
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'