Influencing the properties of dysprosium single-molecule magnets with phosphorus donor ligands
Thomas Pugh; Floriana Tuna; Liviu Ungur; David Collison; Eric J.L. McInnes; Liviu F. Chibotaru; Richard A. Layfield; Nature Communications 6 (2015) 7492–; doi:10.1038/ncomms8492

data_1548185
_publ_section_title
;
 Influencing the properties of dysprosium single-molecule magnets with
 phosphorus donor ligands
;
_journal_name_full               'Nature Communications'
_journal_page_first              7492
_journal_paper_doi               10.1038/ncomms8492
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C63 H75 Dy3 P3, C7 H8'
_chemical_formula_sum            'C70 H83 Dy3 P3'
_chemical_formula_weight         1504.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 103.258(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.8907(6)
_cell_length_b                   18.6253(8)
_cell_length_c                   23.5996(9)
_cell_measurement_reflns_used    8304
_cell_measurement_temperature    150.06(14)
_cell_measurement_theta_max      26.4460
_cell_measurement_theta_min      3.4330
_cell_volume                     6370.8(5)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.06(14)
_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  -94.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7892  178.0000  -60.0000 60

  2 omega   -7.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -99.0000 -120.0000 73

  3 omega   -1.00   52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -77.0000  120.0000 53

  4 omega   35.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -99.0000   30.0000 29

  5 omega  -32.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   19.0000  120.0000 127

  6 omega  -48.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -57.0000  -60.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0034034000
_diffrn_orient_matrix_UB_12      0.0374309000
_diffrn_orient_matrix_UB_13      0.0045719000
_diffrn_orient_matrix_UB_21      0.0486100000
_diffrn_orient_matrix_UB_22      0.0019656000
_diffrn_orient_matrix_UB_23      0.0100980000
_diffrn_orient_matrix_UB_31      0.0045020000
_diffrn_orient_matrix_UB_32      0.0066284000
_diffrn_orient_matrix_UB_33      -0.0288312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25068
_diffrn_reflns_point_group_measured_fraction_full 0.740
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49085
_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
;
;
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.386
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
;
 Flack x determined using 2335 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         9579
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+6.6100P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.475
_reflns_Friedel_fraction_full    0.483
_reflns_Friedel_fraction_max     0.475
_reflns_number_gt                8511
_reflns_number_total             9579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8492-s3.cif
_cod_data_source_block           2
_cod_original_cell_volume        6370.8(4)
_cod_database_code               1548185
_chemical_oxdiff_formula         Dy3P3C80H128
_cell_oxdiff_angle_alpha         90.007(4)
_cell_oxdiff_angle_beta          103.211(4)
_cell_oxdiff_angle_gamma         89.937(4)
_cell_oxdiff_length_a            14.8882(6)
_cell_oxdiff_length_b            18.6343(9)
_cell_oxdiff_length_c            23.5878(10)
_cell_oxdiff_measurement_reflns_used 8305
_cell_oxdiff_volume              6370.8(5)
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H22(0.037) H33(0.046) H28(0.037) H34(0.041) H21(0.056) H2(0.04)
 H16(0.04) H26(0.04) H14(0.034) H4(0.042) H27(0.04) H1(0.047) H19(0.045)
 H3(0.036) H25(0.044) H13(0.038) H15(0.038) H31(0.046) H50(0.046) H48(0.055)
 H52A(0.072) H52B(0.072) H52C(0.072) H41(0.069) H10(0.048) H57(0.063) H9(0.048)
 H32(0.049) H20(0.058) H8(0.056) H7(0.068) H54A(0.083) H54B(0.083) H54C(0.083)
 H53A(0.122) H53B(0.122) H53C(0.122) H39(0.07) H61A(0.128) H61B(0.128)
 H61C(0.128) H63A(0.156) H63B(0.156) H63C(0.156) H43A(0.124) H43B(0.124)
 H43C(0.124) H65(0.118) H64(0.109) H67(0.125) H66(0.106) H30A(0.077)
 H30B(0.077) H30C(0.077) H6A(0.082) H6B(0.082) H6C(0.082) H36A(0.104)
 H36B(0.104) H36C(0.104) H45A(0.123) H45B(0.123) H45C(0.123) H59(0.083)
 H44A(0.123) H44B(0.123) H44C(0.123) H24A(0.075) H24B(0.075) H24C(0.075)
 H12A(0.097) H12B(0.097) H12C(0.097) H18A(0.094) H18B(0.094) H18C(0.094)
 H70A(0.16) H70B(0.16) H70C(0.16) H68(0.116) H62A(0.184) H62B(0.184) H62C(0.184)
 Fixed X: H22(-0.0197) H33(-0.2448) H28(-0.5285) H34(-0.2794) H21(-0.0745) H2(-
 0.4676) H16(-0.4565) H26(-0.5411) H14(-0.3259) H4(-0.3681) H27(-0.4986) H1(-
 0.3897) H19(-0.1863) H3(-0.4536) H25(-0.6083) H13(-0.31) H15(-0.4115) H31(-
 0.5154) H50(-0.047) H48(-0.2458) H52A(-0.3709) H52B(-0.373) H52C(-0.4204)
 H41(0.1546) H10(-0.1381) H57(-0.0832) H9(-0.0481) H32(-0.3899) H20(-0.174) H8(-
 0.0947) H7(-0.219) H54A(-0.1497) H54B(-0.1231) H54C(-0.052) H53A(-0.0187)
 H53B(-0.0871) H53C(-0.1045) H39(0.0646) H61A(-0.1032) H61B(-0.041) H61C(-
 0.1135) H63A(-0.4124) H63B(-0.451) H63C(-0.448) H43A(-0.1338) H43B(-0.0849)
 H43C(-0.1608) H65(0.0655) H64(0.2048) H67(0.1932) H66(0.0654) H30A(-0.6283)
 H30B(-0.6915) H30C(-0.5946) H6A(-0.2569) H6B(-0.3536) H6C(-0.2975) H36A(-
 0.5307) H36B(-0.4596) H36C(-0.4417) H45A(-0.0562) H45B(0.0411) H45C(0.0324)
 H59(-0.3279) H44A(0.25) H44B(0.2251) H44C(0.2587) H24A(-0.1472) H24B(-0.0539)
 H24C(-0.0549) H12A(-0.3272) H12B(-0.2472) H12C(-0.2992) H18A(-0.341) H18B(-
 0.4462) H18C(-0.4114) H70A(0.363) H70B(0.4185) H70C(0.3849) H68(0.3337) H62A(-
 0.1039) H62B(-0.2037) H62C(-0.1602)
 Fixed Y: H22(-0.5833) H33(-0.4384) H28(-0.379) H34(-0.5686) H21(-0.6485) H2(-
 0.2632) H16(-0.6162) H26(-0.5917) H14(-0.5351) H4(-0.3987) H27(-0.4989) H1(-
 0.1906) H19(-0.7432) H3(-0.3922) H25(-0.5365) H13(-0.6677) H15(-0.5019) H31(-
 0.4619) H50(-0.6609) H48(-0.8057) H52A(-0.8052) H52B(-0.7536) H52C(-0.7306)
 H41(-0.435) H10(-0.2351) H57(-0.2641) H9(-0.2984) H32(-0.3724) H20(-0.7484)
 H8(-0.248) H7(-0.1624) H54A(-0.5229) H54B(-0.5487) H54C(-0.556) H53A(-0.7754)
 H53B(-0.8393) H53C(-0.7855) H39(-0.4287) H61A(-0.3993) H61B(-0.334) H61C(-
 0.3648) H63A(-0.244) H63B(-0.2118) H63C(-0.2952) H43A(-0.4747) H43B(-0.4069)
 H43C(-0.3977) H65(-0.428) H64(-0.433) H67(-0.5033) H66(-0.4557) H30A(-0.3985)
 H30B(-0.3725) H30C(-0.3371) H6A(-0.2396) H6B(-0.2366) H6C(-0.3085) H36A(-
 0.6034) H36B(-0.6273) H36C(-0.6458) H45A(-0.4477) H45B(-0.4126) H45C(-0.4959)
 H59(-0.1748) H44A(-0.3828) H44B(-0.4397) H44C(-0.4649) H24A(-0.6241) H24B(-
 0.6666) H24C(-0.5858) H12A(-0.1211) H12B(-0.0862) H12C(-0.1537) H18A(-0.7764)
 H18B(-0.7689) H18C(-0.7564) H70A(-0.4484) H70B(-0.4481) H70C(-0.5209) H68(-
 0.5032) H62A(-0.1847) H62B(-0.1708) H62C(-0.118)
 Fixed Z: H22(-0.3035) H33(-0.068) H28(-0.2672) H34(-0.0684) H21(-0.2244) H2(-
 0.3227) H16(-0.3345) H26(-0.2465) H14(-0.4514) H4(-0.4271) H27(-0.3094) H1(-
 0.3852) H19(-0.3763) H3(-0.3482) H25(-0.1735) H13(-0.453) H15(-0.3783) H31(-
 0.0723) H50(-0.0588) H48(-0.0959) H52A(-0.1709) H52B(-0.2236) H52C(-0.1736)
 H41(-0.263) H10(-0.2016) H57(-0.0367) H9(-0.2614) H32(-0.0682) H20(-0.2732)
 H8(-0.3622) H7(-0.3642) H54A(-0.1162) H54B(-0.1734) H54C(-0.1134) H53A(-
 0.0132) H53B(-0.0333) H53C(0.0141) H39(-0.4335) H61A(-0.0988) H61B(-0.1072)
 H61C(-0.1606) H63A(-0.2027) H63B(-0.1517) H63C(-0.1599) H43A(-0.46) H43B(-
 0.4785) H43C(-0.4428) H65(-0.0038) H64(0.0638) H67(-0.1223) H66(-0.1023) H30A(-
 0.138) H30B(-0.1969) H30C(-0.1735) H6A(-0.4551) H6B(-0.4987) H6C(-0.4898)
 H36A(-0.0915) H36B(-0.0349) H36C(-0.0962) H45A(-0.2259) H45B(-0.2034) H45C(-
 0.2124) H59(-0.0642) H44A(-0.3451) H44B(-0.3952) H44C(-0.3304) H24A(-0.4477)
 H24B(-0.4355) H24C(-0.4173) H12A(-0.2898) H12B(-0.243) H12C(-0.227) H18A(-
 0.3771) H18B(-0.4065) H18C(-0.3393) H70A(0.0882) H70B(0.0392) H70C(0.0605)
 H68(-0.059) H62A(0.0309) H62B(0.0396) H62C(0.0017)
;
_shelx_res_checksum              61355
_shelx_hkl_checksum              13695