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_1549771
_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 Y, C8 H8'
_chemical_formula_sum            'C20 H32 P Si2 Y'
_chemical_formula_weight         448.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-04-10 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.180(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2388(7)
_cell_length_b                   10.8568(5)
_cell_length_c                   14.2170(8)
_cell_measurement_reflns_used    8024
_cell_measurement_temperature    179.9(3)
_cell_measurement_theta_max      27.1120
_cell_measurement_theta_min      3.7930
_cell_volume                     2342.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_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     23.00  88.00   0.50    2.00    --   -1.70  19.00 -30.00  130
  2  \w      5.00  87.00   0.50    2.00    --   -1.70  57.00-120.00  164
  3  \w      0.00  28.00   0.50    2.00    --   -1.70 -77.00  30.00   56
  4  \w    -19.00   6.00   0.50    2.00    --   -1.70 -82.00 120.00   50
  5  \w    -31.00  30.00   0.50    2.00    --   -1.70 -82.00 -90.00  122
  6  \w    -20.00   6.00   0.50    2.00    --   -1.70 -82.00-150.00   52
  7  \w     -1.00  30.00   0.50    2.00    --   -1.70 -82.00-180.00   62
  8  \w    -18.00  48.00   0.50    2.00    --   -1.70  37.00  60.00  132
  9  \w     66.00  91.00   0.50    2.00    --    1.90  57.00-120.00   50
 10  \w    -20.00  12.00   0.50    2.00    --    1.90  57.00-120.00   64
 11  \w    -30.00  31.00   0.50    2.00    --    1.90 -82.00-120.00  122
 12  \w     42.00  67.00   0.50    2.00    --    1.90  19.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0261723000
_diffrn_orient_matrix_UB_12      -0.0480960000
_diffrn_orient_matrix_UB_13      0.0214709000
_diffrn_orient_matrix_UB_21      -0.0246601000
_diffrn_orient_matrix_UB_22      0.0023208000
_diffrn_orient_matrix_UB_23      0.0399499000
_diffrn_orient_matrix_UB_31      -0.0298571000
_diffrn_orient_matrix_UB_32      -0.0441638000
_diffrn_orient_matrix_UB_33      -0.0212571000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47306
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         30.282
_diffrn_reflns_theta_min         3.589
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6315
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0253P)^2^+1.4404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4926
_reflns_number_total             6315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01626g2.cif
_cod_data_source_block           2_reducted
_cod_depositor_comments
'Adding full bibliography for 1549767--1549771.cif.'
_cod_database_code               1549771
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C20 H32 Si2 P1 Y1'
_reflns_odcompleteness_completeness 99.63
_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. Restrained distances
 C1-C2 \\sim C2-C3
 with sigma of 0.015
 C2-C3 \\sim C3-C4
 with sigma of 0.015
 C3-C4 \\sim C4-C5
 with sigma of 0.015
 C4-C5 \\sim C5-C6
 with sigma of 0.015
 C5-C6 \\sim C6-C7
 with sigma of 0.015
 C6-C7 \\sim C7-C8
 with sigma of 0.015
 C7-C8 \\sim C8-C1
 with sigma of 0.015
 C8-C1 \\sim C1-C2
 with sigma of 0.015
 C1B-C2B \\sim C2B-C3B
 with sigma of 0.015
 C2B-C3B \\sim C3B-C4B
 with sigma of 0.015
 C3B-C4B \\sim C4B-C5B
 with sigma of 0.015
 C4B-C5B \\sim C5B-C6B
 with sigma of 0.015
 C5B-C6B \\sim C6B-C7B
 with sigma of 0.015
 C6B-C7B \\sim C7B-C8B
 with sigma of 0.015
 C7B-C8B \\sim C8B-C1B
 with sigma of 0.015
 C8B-C1B \\sim C1B-C2B
 with sigma of 0.015
 C7B-C6B \\sim C5B-C4B
 with sigma of 0.02
 C2-C1 \\sim C7-C6
 with sigma of 0.02
 C8-C1 \\sim C7-C6
 with sigma of 0.015
3. Restrained planarity
 C5, C4, C7, C3, C1, C8, C6, C2
 with sigma of 0.1
 C3B, C2B, C6B, C5B, C7B, C4B, C8B, C1B
 with sigma of 0.1
4. Rigid bond restraints
 C5, C4, C3, C2, C1, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4B, C5B, C6B, C7B, C8B, C3B, C2B, C1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1B, C2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2B, C3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3B, C4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4B, C5B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5B, C6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6B, C7B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7B, C8B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8B, C1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim C6 \\sim C7 \\sim C8: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim C3B \\sim C2B \\sim C1B:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3 \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C4 \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C5 \\sim C6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C6 \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 \\sim C8: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1B \\sim C2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C2B \\sim C3B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C3B \\sim C4B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C4B \\sim C5B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C5B \\sim C6B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C6B \\sim C7B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C7B \\sim C8B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C8B \\sim C1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C4B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C7B)
\\sim Ueq, Uanis(C8B) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C2B) \\sim Ueq,
Uanis(C1B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
6. Others
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(H2B)=
 Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C8B)=Sof(H8B)=Sof(C1B)=Sof(H1B)=1-
 FVAR(1)
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(H4)=Sof(C2)=Sof(H2)=Sof(C8)=Sof(H8)=Sof(C5)=Sof(H5)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C1(H1), C3(H3), C4(H4), C2(H2), C8(H8), C5(H5), C6B(H6B),
 C7B(H7B), C3B(H3B), C2B(H2B), C4B(H4B), C5B(H5B), C8B(H8B), C1B(H1B)
7.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C14(H14A,H14B,
 H14C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              98466
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.813