A soft phosphorus atom to "harden" an erbium(iii) single-ion magnet.
Chen, Shi-Ming; Xiong, Jin; Zhang, Yi-Quan; Yuan, Qiong; Wang, Bing-Wu; Gao, Song; Chemical science 9 (2018) 7540–7545; doi:10.1039/c8sc01626g

data_1549767
_publ_section_title
;
 A soft phosphorus atom to &quot;harden&quot; an erbium(iii) single-ion
 magnet.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              7540
_journal_page_last               7545
_journal_paper_doi               10.1039/c8sc01626g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C12 H24 P Si2 Tb, C8 H8'
_chemical_formula_sum            'C20 H32 P Si2 Tb'
_chemical_formula_weight         518.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-05-13
_audit_creation_method
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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_audit_update_record
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2018-04-10 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   18.8787(12)
_cell_length_c                   9.3269(5)
_cell_measurement_reflns_used    3935
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.2900
_cell_measurement_theta_min      3.8120
_cell_volume                     2259.4(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_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
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega   35.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  178.0000  -30.0000 69

  2 omega  -60.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -77.0000  -30.0000 93

  3 omega  -10.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   57.0000   90.0000 93

  4 omega   -8.00   27.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7128  -99.0000   90.0000 35
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_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0055727000
_diffrn_orient_matrix_UB_12      -0.0368577000
_diffrn_orient_matrix_UB_13      0.0126431000
_diffrn_orient_matrix_UB_21      -0.0119939000
_diffrn_orient_matrix_UB_22      0.0052954000
_diffrn_orient_matrix_UB_23      0.0734678000
_diffrn_orient_matrix_UB_31      -0.0536626000
_diffrn_orient_matrix_UB_32      -0.0050101000
_diffrn_orient_matrix_UB_33      -0.0150870000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         30.293
_diffrn_reflns_theta_min         3.172
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88837
_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_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0100P)^2^+2.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2197
_reflns_number_total             3273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01626g2.cif
_cod_data_source_block           1_reducted
_cod_depositor_comments
'Adding full bibliography for 1549767--1549771.cif.'
_cod_database_code               1549767
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C20 H32 Si2 P1 Tb1'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C1(H1), C4(H4)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              9896
_olex2_submission_special_instructions 'No special instructions were received'