#------------------------------------------------------------------------------
#$Date: 2022-06-29 12:43:46 +0300 (Wed, 29 Jun 2022) $
#$Revision: 276399 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/97/1549769.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1549769
loop_
_publ_author_name
'Chen, Shi-Ming'
'Xiong, Jin'
'Zhang, Yi-Quan'
'Yuan, Qiong'
'Wang, Bing-Wu'
'Gao, Song'
_publ_section_title
;
 A soft phosphorus atom to "harden" 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 Dy P Si2, C8 H8'
_chemical_formula_sum            'C20 H32 Dy P Si2'
_chemical_formula_weight         522.10
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-05-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8248(7)
_cell_length_b                   18.9114(12)
_cell_length_c                   9.3047(4)
_cell_measurement_reflns_used    3359
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.6090
_cell_measurement_theta_min      3.4190
_cell_volume                     2256.7(2)
_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, 2015)'
_computing_structure_solution
;
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 0.929
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -9.00   80.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   57.0000   60.0000 89

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.00   10.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -57.0000  120.0000 89

#__ type_ start__ end____ width___ exp.time_
  3 omega  -35.00   59.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566   57.0000  -90.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0207453000
_diffrn_orient_matrix_UB_12      -0.0334769000
_diffrn_orient_matrix_UB_13      -0.0190504000
_diffrn_orient_matrix_UB_21      -0.0230115000
_diffrn_orient_matrix_UB_22      0.0029454000
_diffrn_orient_matrix_UB_23      -0.0690890000
_diffrn_orient_matrix_UB_31      0.0457998000
_diffrn_orient_matrix_UB_32      0.0166495000
_diffrn_orient_matrix_UB_33      -0.0260361000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            15778
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         30.283
_diffrn_reflns_theta_min         3.174
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84688
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0324
_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/[σ²(Fo²)+(0.0100P)²+2.3860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2126
_reflns_number_total             3233
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc01626g2.cif
_cod_data_source_block           1_reducted_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1549767--1549771.cif.'
_cod_database_code               1549769
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C20 H32 Si2 P1 Dy1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.59
_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:
 C1(H1), C4(H4)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Dy1 Dy 0.19907(2) 0.2500 0.49946(3) 0.02352(7) Uani 1 2 d S T P
P1 P 0.12953(10) 0.2500 0.79125(13) 0.0206(3) Uani 1 2 d S T P
Si1 Si 0.08087(8) 0.41234(5) 0.73981(11) 0.0260(2) Uani 1 1 d . . .
C6 C 0.0060(3) 0.28739(17) 0.5788(3) 0.0226(8) Uani 1 1 d . . .
C10 C 0.1592(3) 0.4179(2) 0.9076(4) 0.0442(11) Uani 1 1 d . . .
H10A H 0.1222 0.3938 0.9856 0.066 Uiso 1 1 calc GR . .
H10B H 0.1698 0.4677 0.9332 0.066 Uiso 1 1 calc GR . .
H10C H 0.2270 0.3952 0.8924 0.066 Uiso 1 1 calc GR . .
C5 C 0.0710(3) 0.31741(17) 0.6856(3) 0.0202(7) Uani 1 1 d . . .
C9 C 0.1439(3) 0.4682(2) 0.6001(4) 0.0431(11) Uani 1 1 d . . .
H9A H 0.1430 0.5178 0.6310 0.065 Uiso 1 1 calc GR . .
H9B H 0.1057 0.4635 0.5094 0.065 Uiso 1 1 calc GR . .
H9C H 0.2162 0.4528 0.5864 0.065 Uiso 1 1 calc GR . .
C1 C 0.3855(3) 0.2872(2) 0.4506(4) 0.0368(10) Uani 1 1 d . . .
H1 H 0.4413 0.3064 0.5051 0.044 Uiso 1 1 calc R . .
C2 C 0.3223(3) 0.3396(2) 0.3889(4) 0.0376(10) Uani 1 1 d . . .
C3 C 0.2319(4) 0.3396(3) 0.3034(4) 0.0405(11) Uani 1 1 d . . .
C8 C -0.0520(3) 0.4487(2) 0.7786(4) 0.0424(11) Uani 1 1 d . . .
H8A H -0.0856 0.4199 0.8529 0.064 Uiso 1 1 calc GR . .
H8B H -0.0941 0.4475 0.6908 0.064 Uiso 1 1 calc GR . .
H8C H -0.0457 0.4976 0.8124 0.064 Uiso 1 1 calc GR . .
C4 C 0.1694(3) 0.2130(2) 0.2426(4) 0.0453(12) Uani 1 1 d . . .
H4 H 0.1134 0.1939 0.1882 0.054 Uiso 1 1 calc R . .
C7 C -0.0620(3) 0.3296(2) 0.4768(4) 0.0380(10) Uani 1 1 d . . .
H7A H -0.0551 0.3105 0.3794 0.057 Uiso 1 1 calc GR . .
H7B H -0.0399 0.3792 0.4776 0.057 Uiso 1 1 calc GR . .
H7C H -0.1349 0.3263 0.5076 0.057 Uiso 1 1 calc GR . .
H3 H 0.210(3) 0.386(2) 0.294(4) 0.036(12) Uiso 1 1 d . . .
H2 H 0.341(3) 0.384(2) 0.415(4) 0.044(13) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C6 Dy1 P1 56.62(7) 8_565 .
C6 Dy1 P1 56.62(7) . .
C6 Dy1 C6 30.61(14) . 8_565
C6 Dy1 C5 52.20(10) . 8_565
C6 Dy1 C5 30.50(10) 8_565 8_565
C6 Dy1 C5 52.20(10) 8_565 .
C6 Dy1 C5 30.50(10) . .
C5 Dy1 P1 37.10(7) 8_565 .
C5 Dy1 P1 37.10(7) . .
C5 Dy1 C5 56.22(14) . 8_565
C5 P1 Dy1 66.80(11) 8_565 .
C5 P1 Dy1 66.80(11) . .
C5 P1 C5 91.8(2) . 8_565
C10 Si1 C5 108.51(17) . .
C10 Si1 C9 108.6(2) . .
C10 Si1 C8 108.0(2) . .
C5 Si1 C8 110.06(17) . .
C9 Si1 C5 112.73(17) . .
C9 Si1 C8 108.77(19) . .
C6 C6 Dy1 74.70(7) 8_565 .
C6 C6 C5 113.63(19) 8_565 .
C6 C6 C7 121.8(2) 8_565 .
C5 C6 Dy1 75.80(19) . .
C5 C6 C7 124.5(3) . .
C7 C6 Dy1 119.9(2) . .
P1 C5 Dy1 76.10(12) . .
P1 C5 Si1 120.78(18) . .
Si1 C5 Dy1 125.76(15) . .
C6 C5 Dy1 73.70(18) . .
C6 C5 P1 110.5(2) . .
C6 C5 Si1 127.9(2) . .
C2 C1 C1 134.9(2) . 8_565
C1 C2 C3 135.0(4) . .
C4 C3 C2 134.6(4) 8_565 .
C3 C4 C4 135.4(3) 8_565 8_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 P1 2.8577(12) .
Dy1 C6 2.679(3) .
Dy1 C6 2.679(3) 8_565
Dy1 C5 2.706(3) .
Dy1 C5 2.706(3) 8_565
P1 C5 1.776(3) .
P1 C5 1.776(3) 8_565
Si1 C10 1.860(4) .
Si1 C5 1.869(3) .
Si1 C9 1.860(4) .
Si1 C8 1.872(4) .
C6 C6 1.414(7) 8_565
C6 C5 1.416(4) .
C6 C7 1.515(5) .
C1 C1 1.406(8) 8_565
C1 C2 1.404(5) .
C2 C3 1.406(6) .
C3 C4 1.396(6) 8_565
C4 C3 1.396(6) 8_565
C4 C4 1.399(8) 8_565
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-06-29T12:40:00+03:00
;
 Removed the '_chemical_name_systematic' data item that had an incorrect value.
;
