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_7032300
_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 La2 N2 O42 P4, 2(H2 O), 0.57(C4 H10 O), 1.43(C4 H9 O)'
_chemical_formula_sum            'C98 H210 Cr6 La2 N2 O46 P4'
_chemical_formula_weight         2866.37
_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                100.081(3)
_cell_angle_beta                 100.916(3)
_cell_angle_gamma                107.940(3)
_cell_formula_units_Z            1
_cell_length_a                   13.7609(5)
_cell_length_b                   13.9671(5)
_cell_length_c                   23.3521(8)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.6330
_cell_measurement_theta_min      3.1170
_cell_volume                     4059.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
  1 omega  -19.00   12.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -77.0000   60.0000 31

  2 omega  -33.00   -6.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -57.0000   90.0000 27

  3 omega  -88.00   -5.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -57.0000  150.0000 83

  4 omega  -89.00  -60.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -77.0000  -90.0000 29

  5 omega  -39.00   -4.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -77.0000  -90.0000 35

  6 omega  -81.00  -35.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -77.0000   60.0000 46

  7 omega  -66.00    0.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -37.0000  150.0000 66

  8 omega  -85.00  -43.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -57.0000  -90.0000 42

  9 omega  -73.00  -39.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866  -57.0000   90.0000 34

 10 omega  -20.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6554  -99.0000   30.0000 83

 11 omega  -29.00   17.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6554  -57.0000  -60.0000 46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0339326000
_diffrn_orient_matrix_UB_12      0.0118350000
_diffrn_orient_matrix_UB_13      -0.0223450000
_diffrn_orient_matrix_UB_21      0.0195928000
_diffrn_orient_matrix_UB_22      0.0525945000
_diffrn_orient_matrix_UB_23      0.0167841000
_diffrn_orient_matrix_UB_31      0.0401545000
_diffrn_orient_matrix_UB_32      0.0115210000
_diffrn_orient_matrix_UB_33      -0.0154788000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.1090
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40717
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.183
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             1498
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.082
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         18761
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1114P)^2^+9.7113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13130
_reflns_number_total             18761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031804
_cod_data_source_file            c4dt01264j2.cif
_cod_data_source_block           Cr6La2P4
_cod_database_code               7032300
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         Cr6La2P4O52c100h100
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3S(0.044) H66A(0.064) H66B(0.064) H66C(0.064) H67A(0.059)
 H67B(0.059) H67C(0.059) H65A(0.071) H65B(0.071) H65C(0.071) H77A(0.09)
 H77B(0.09) H77C(0.09) H76A(0.074) H76B(0.074) H76C(0.074) H27A(0.069)
 H27B(0.069) H27C(0.069) H37A(0.109) H37B(0.109) H37C(0.109) H75A(0.106)
 H75B(0.106) H75C(0.106) H26A(0.104) H26B(0.104) H26C(0.104) H5S(0.07)
 H47A(0.114) H47B(0.114) H47C(0.114) H4SA(0.047) H4SB(0.047) H5A(0.095)
 H5B(0.095) H5C(0.095) H35A(0.111) H35B(0.111) H35C(0.111) H16A(0.099)
 H16B(0.099) H16C(0.099) H6SA(0.117) H6SB(0.117) H6SC(0.117) H25A(0.128)
 H25B(0.128) H25C(0.128) H45A(0.143) H45B(0.143) H45C(0.143) H55A(0.159)
 H55B(0.159) H55C(0.159) H7A(0.18) H7B(0.18) H7C(0.18) H56A(0.143) H56B(0.143)
 H56C(0.143) H46A(0.116) H46B(0.116) H46C(0.116) H6A(0.178) H6B(0.178)
 H6C(0.178) H1SA(0.045) H1SB(0.045) H2SA(0.065) H2SB(0.065) H31A(0.087)
 H31B(0.087) H36A(0.123) H36B(0.123) H36C(0.123) H7SA(0.123) H7SB(0.123)
 H7SC(0.123) H15A(0.108) H15B(0.108) H15C(0.108) H17A(0.098) H17B(0.098)
 H17C(0.098) H33A(0.16) H33B(0.16) H33C(0.16) H34A(0.308) H34B(0.308)
 H34C(0.308) H57A(0.167) H57B(0.167) H57C(0.167) H32S(0.128) H33D(0.43)
 H33E(0.43) H33F(0.43) H8A(0.169) H34D(0.309) H34E(0.309) H34F(0.309)
 H31C(0.087) H31D(0.087) H16D(0.135) H16E(0.135) H16F(0.135) H17D(0.166)
 H17E(0.166) H17F(0.166) H15D(0.125) H15E(0.125) H15F(0.125) H56D(0.209)
 H56E(0.209) H56F(0.209) H57D(0.204) H57E(0.204) H57F(0.204) H55D(0.207)
 H55E(0.207) H55F(0.207) H41T(0.065) H43T(0.078) H42A(0.065) H42B(0.065)
 H45D(0.099) H45E(0.099) H45F(0.099) H44A(0.184) H44B(0.184) H44C(0.184)
 H22A(0.077) H22B(0.077) H23T(0.088) H25D(0.195) H25E(0.195) H25F(0.195)
 H24A(0.186) H24B(0.186) H24C(0.186) H2(0.106) H1A(0.099) H1B(0.099) H1C(0.099)
 H9A(0.106) H9B(0.106) H10A(0.201) H10B(0.201) H10C(0.201)
 Fixed X: H66A(0.6823) H66B(0.6701) H66C(0.7853) H67A(0.59) H67B(0.5504)
 H67C(0.565) H65A(0.8271) H65B(0.7115) H65C(0.7504) H77A(1.06) H77B(1.037)
 H77C(0.9421) H76A(1.0814) H76B(1.1215) H76C(1.1469) H27A(0.5741) H27B(0.5191)
 H27C(0.6311) H37A(0.9008) H37B(0.8875) H37C(0.8033) H75A(0.8403) H75B(0.9324)
 H75C(0.8931) H26A(0.3625) H26B(0.3563) H26C(0.4073) H5S(0.8178) H47A(1.3014)
 H47B(1.3959) H47C(1.2774) H4SA(0.6393) H4SB(0.6418) H5A(0.7628) H5B(0.6838)
 H5C(0.6923) H35A(0.9108) H35B(0.9451) H35C(0.8288) H16A(0.4044) H16B(0.2795)
 H16C(0.3433) H6SA(0.6684) H6SB(0.7714) H6SC(0.6786) H25A(0.5657) H25B(0.4537)
 H25C(0.4597) H45A(1.344) H45B(1.4603) H45C(1.4061) H55A(0.7178) H55B(0.787)
 H55C(0.8378) H7A(0.5566) H7B(0.6059) H7C(0.6821) H56A(0.8902) H56B(0.8417)
 H56C(0.8051) H46A(1.431) H46B(1.4896) H46C(1.3888) H6A(0.5006) H6B(0.4872)
 H6C(0.4438) H1SA(0.9969) H1SB(1.0957) H2SA(1.1175) H2SB(1.0103) H31A(0.3887)
 H31B(0.4515) H36A(1.0851) H36B(1.099) H36C(1.0683) H7SA(0.8739) H7SB(0.894)
 H7SC(0.7961) H15A(0.3713) H15B(0.2867) H15C(0.4102) H17A(0.2637) H17B(0.2019)
 H17C(0.2692) H33A(0.2924) H33B(0.2555) H33C(0.3757) H34A(0.2518) H34B(0.1792)
 H34C(0.2292) H57A(0.6266) H57B(0.667) H57C(0.5803) H32S(0.3614) H33D(0.4678)
 H33E(0.514) H33F(0.397) H8A(0.4602) H34D(0.2512) H34E(0.3058) H34F(0.3392)
 H31C(0.3649) H31D(0.4262) H16D(0.3581) H16E(0.2461) H16F(0.2912) H17D(0.2855)
 H17E(0.2334) H17F(0.3399) H15D(0.4314) H15E(0.3342) H15F(0.4468) H56D(0.7809)
 H56E(0.7462) H56F(0.6585) H57D(0.5929) H57E(0.677) H57F(0.679) H55D(0.8548)
 H55E(0.8664) H55F(0.894) H41T(0.2948) H43T(0.3619) H42A(0.449) H42B(0.338)
 H45D(0.3662) H45E(0.3636) H45F(0.4651) H44A(0.1832) H44B(0.198) H44C(0.1944)
 H22A(0.2593) H22B(0.2538) H23T(0.0751) H25D(0.2423) H25E(0.135) H25F(0.2177)
 H24A(0.1338) H24B(0.0449) H24C(0.0282) H2(0.0967) H1A(-0.0696) H1B(-0.0521)
 H1C(-0.0902) H9A(0.0279) H9B(0.083) H10A(0.1228) H10B(0.0987) H10C(0.2044)
 Fixed Y: H66A(0.4643) H66B(0.5759) H66C(0.5677) H67A(0.4769) H67B(0.5201)
 H67C(0.4096) H65A(0.677) H65B(0.6842) H65C(0.6411) H77A(0.2042) H77B(0.121)
 H77C(0.1253) H76A(0.3604) H76B(0.2642) H76C(0.3479) H27A(0.627) H27B(0.6778)
 H27C(0.6677) H37A(0.6847) H37B(0.7958) H37C(0.6988) H75A(0.1467) H75B(0.1422)
 H75C(0.2391) H26A(0.4088) H26B(0.5201) H26C(0.4635) H5S(0.0196) H47A(0.6732)
 H47B(0.7828) H47C(0.7789) H4SA(0.0111) H4SB(0.0404) H5A(-0.0403) H5B(-0.1586)
 H5C(-0.0851) H35A(0.8944) H35B(0.8488) H35C(0.7943) H16A(0.259) H16B(0.2)
 H16C(0.281) H6SA(-0.1295) H6SB(-0.145) H6SC(-0.1419) H25A(0.5728) H25B(0.5853)
 H25C(0.4725) H45A(0.893) H45B(0.8928) H45C(0.8547) H55A(0.4898) H55B(0.4561)
 H55C(0.5034) H7A(-0.0404) H7B(-0.1302) H7C(-0.0109) H56A(0.3459) H56B(0.3135)
 H56C(0.2323) H46A(0.6791) H46B(0.7195) H46C(0.6143) H6A(-0.1169) H6B(-0.1975)
 H6C(-0.1038) H1SA(0.7416) H1SB(0.7424) H2SA(0.5453) H2SB(0.4974) H31A(0.2271)
 H31B(0.189) H36A(0.7676) H36B(0.8326) H36C(0.8772) H7SA(0.1236) H7SB(0.0162)
 H7SC(0.0327) H15A(-0.0111) H15B(0.0159) H15C(0.0668) H17A(0.1571) H17B(0.0742)
 H17C(0.0428) H33A(0.0853) H33B(-0.0321) H33C(0.0266) H34A(0.1182) H34B(0.0316)
 H34C(0.1502) H57A(0.2087) H57B(0.3009) H57C(0.3009) H32S(0.0244) H33D(-0.001)
 H33E(0.1223) H33F(0.0562) H8A(0.0567) H34D(-0.0341) H34E(-0.039) H34F(-0.0869)
 H31C(0.1596) H31D(0.2299) H16D(0.2967) H16E(0.2095) H16F(0.222) H17D(0.048)
 H17E(0.014) H17F(-0.0051) H15D(0.0981) H15E(0.1322) H15F(0.2187) H56D(0.2126)
 H56E(0.2315) H56F(0.1854) H57D(0.3383) H57E(0.3877) H57F(0.4526) H55D(0.4767)
 H55E(0.4141) H55F(0.3801) H41T(0.3009) H43T(0.2207) H42A(0.3825) H42B(0.3998)
 H45D(0.4036) H45E(0.2983) H45F(0.3661) H44A(0.203) H44B(0.1982) H44C(0.3023)
 H22A(0.5959) H22B(0.6467) H23T(0.6365) H25D(0.7872) H25E(0.7979) H25F(0.7808)
 H24A(0.5882) H24B(0.6393) H24C(0.5283) H2(0.1399) H1A(0.0759) H1B(0.0025)
 H1C(0.0967) H9A(0.275) H9B(0.2589) H10A(0.0353) H10B(0.1135) H10C(0.1519)
 Fixed Z: H66A(1.0286) H66B(1.0386) H66C(1.0493) H67A(0.8783) H67B(0.9341)
 H67C(0.9261) H65A(0.9753) H65B(0.9651) H65C(0.9088) H77A(0.8669) H77B(0.8048)
 H77C(0.8344) H76A(0.7589) H76B(0.7575) H76C(0.8197) H27A(0.83) H27B(0.7832)
 H27C(0.7806) H37A(0.7006) H37B(0.712) H37C(0.7245) H75A(0.7397) H75B(0.7077)
 H75C(0.7108) H26A(0.7246) H26B(0.7504) H26C(0.7951) H5S(0.9079) H47A(0.8111)
 H47B(0.8272) H47C(0.8239) H4SA(0.8801) H4SB(0.9499) H5A(0.7412) H5B(0.7213)
 H5C(0.7843) H35A(0.8167) H35B(0.8724) H35C(0.8279) H16A(0.9095) H16B(0.883)
 H16C(0.8506) H6SA(0.9484) H6SB(0.9324) H6SC(0.8806) H25A(0.6745) H25B(0.6736)
 H25C(0.652) H45A(0.9334) H45B(0.9337) H45C(0.9845) H55A(0.5989) H55B(0.5569)
 H55C(0.6278) H7A(0.6243) H7B(0.6251) H7C(0.6449) H56A(0.6312) H56B(0.5598)
 H56C(0.5989) H46A(0.9576) H46B(0.9087) H46C(0.8886) H6A(0.76) H6B(0.6986)
 H6C(0.6969) H1SA(1.0092) H1SB(1.0411) H2SA(0.7812) H2SB(0.7531) H31A(0.6612)
 H31B(0.6178) H36A(0.7715) H36B(0.8381) H36C(0.7813) H7SA(1.0068) H7SB(1.0049)
 H7SC(1.0274) H15A(0.835) H15B(0.8671) H15C(0.9005) H17A(0.7586) H17B(0.7906)
 H17C(0.7466) H33A(0.5448) H33B(0.5509) H33C(0.5513) H34A(0.6911) H34B(0.6309)
 H34C(0.6287) H57A(0.5441) H57B(0.5125) H57C(0.5495) H32S(0.6549) H33D(0.5387)
 H33E(0.5481) H33F(0.5066) H8A(0.6229) H34D(0.5635) H34E(0.6293) H34F(0.572)
 H31C(0.6646) H31D(0.6271) H16D(0.8556) H16E(0.8483) H16F(0.7907) H17D(0.7611)
 H17E(0.8135) H17F(0.8067) H15D(0.9155) H15E(0.9266) H15F(0.9342) H56D(0.5952)
 H56E(0.5299) H56F(0.5639) H57D(0.5629) H57E(0.5276) H57F(0.5917) H55D(0.6333)
 H55E(0.5722) H55F(0.6335) H41T(0.5899) H43T(0.4708) H42A(0.5462) H42B(0.5363)
 H45D(0.4296) H45E(0.3881) H45F(0.4427) H44A(0.4718) H44B(0.4051) H44C(0.4447)
 H22A(0.6299) H22B(0.6959) H23T(0.6492) H25D(0.6787) H25E(0.645) H25F(0.6081)
 H24A(0.5422) H24B(0.5449) H24C(0.5594) H2(0.5458) H1A(0.6047) H1B(0.5498)
 H1C(0.539) H9A(0.5922) H9B(0.6546) H10A(0.6199) H10B(0.6693) H10C(0.6475)
;
_shelx_res_checksum              64393
_olex2_submission_special_instructions 'No special instructions were received'