Enhancing the energy barrier by replacing the counterions in two holmium(iii)-pentagonal bipyramidal single-ion magnets.
Li, Lei-Lei; Su, Hong-Dan; Liu, Shuang; Wang, Wen-Zhen; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6703–6709; doi:10.1039/d0dt00905a

data_7704187
_publ_section_title
;
 Enhancing the energy barrier by replacing the counterions in two
 holmium(iii)-pentagonal bipyramidal single-ion magnets.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6703
_journal_page_last               6709
_journal_paper_doi               10.1039/d0dt00905a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C12 H46 Ho N6 O7 P2, 3(Br), 2(C6 H18 N3 O P)'
_chemical_formula_sum            'C24 H82 Br3 Ho N12 O9 P4'
_chemical_formula_weight         1211.55
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-09 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.623(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2772(6)
_cell_length_b                   15.5914(4)
_cell_length_c                   22.7448(7)
_cell_measurement_reflns_used    5098
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.6890
_cell_measurement_theta_min      3.7050
_cell_volume                     5191.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  38.00   1.00    3.00    --   18.94  37.00-150.00   42
  2  \w      7.00  60.00   1.00    3.00    --   18.94 -99.00-150.00   53
  3  \w     19.00  61.00   1.00    3.00    --   18.94 -99.00 -60.00   42
  4  \w    -47.00 -22.00   1.00    3.00    --  -20.11  77.00 150.00   25
  5  \w    -90.00  19.00   1.00    3.00    --  -20.11 -19.00-150.00  109
  6  \w     -1.00  45.00   1.00    3.00    --  -20.11  77.00 150.00   46
  7  \w    -90.00  10.00   1.00    3.00    --  -20.11 -77.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0263133000
_diffrn_orient_matrix_UB_12      -0.0379778000
_diffrn_orient_matrix_UB_13      -0.0019950000
_diffrn_orient_matrix_UB_21      -0.0265719000
_diffrn_orient_matrix_UB_22      0.0119130000
_diffrn_orient_matrix_UB_23      -0.0298718000
_diffrn_orient_matrix_UB_31      0.0308256000
_diffrn_orient_matrix_UB_32      -0.0220033000
_diffrn_orient_matrix_UB_33      -0.0127854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17040
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.045
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.006
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 2906 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.012(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8612
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0420
_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^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.865
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                7604
_reflns_number_total             8612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00905a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7704187--7704188.cif.'
_cod_database_code               7704187
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N Br Ho'
_chemical_oxdiff_usercomment     LLL
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.501
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H32B-O41
 2 with sigma of 0.02
 C16A-N51 = C16B-N51 = C15A-N51 = C15B-N51
 1.47 with sigma of 0.01
 N0AA-C2AA = N0AA-C17 = N0AA-C6 = N0AA-C18
 1.47 with sigma of 0.02
 H14A-H6C
 2.4 with sigma of 0.02
 H14A-H6A
 2.4 with sigma of 0.02
 H0AC_$1-H15D
 2.2 with sigma of 0.02
 H58B-H29A
 2.2 with sigma of 0.02
 H29B-O41
 2 with sigma of 0.02
 H58B-O50
 2 with sigma of 0.02
3. Rigid bond restraints
 N51, C16B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N51, C15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2AA, N0AA, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C15B) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16B) \\sim Ueq,
Uanis(C16A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C16B) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(C15A) \\sim Ueq,
Uanis(C16A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C16B) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C16B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2AA) \\sim Ueq, Uanis(N0AA) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=1-FVAR(1)
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-
 FVAR(2)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 FVAR(2)
6.a Rotating group:
 O29(H29A,H29B), O32(H32A,H32B), O58(H58A,H58B), O70(H70A,H70B), O76(H76A,H76B)
6.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C44(H44A,H44B,H44C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C), C71(H71A,
 H71B,H71C), C80(H80A,H80B,H80C), C91(H91A,H91B,H91C), C95(H95A,H95B,H95C),
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15B(H15A,H15B,H15C), C16B(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C1AA(H1AA,H1AB,
 H1AC), C0AA(H0AA,H0AB,H0AC), C16A(H16D,H16E,H16F), C15A(H15D,H15E,H15F),
 C6(H6A,H6B,H6C), C2AA(H2AA,H2AB,H2AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.667
_oxdiff_exptl_absorpt_empirical_full_min 0.445