Rare earth 3-(4′-hydroxyphenyl)propionate complexes
Deacon, Glen B.; Junk, Peter C.; Lee, Winnie W.; Forsyth, Maria; Wang, Jun; New J. Chem. 39 (2015) 7688–; doi:10.1039/C5NJ00787A

data_7055007
_publ_section_title
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 Rare earth 3-(4&#x2032;-hydroxyphenyl)propionate complexes
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_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              7688
_journal_paper_doi               10.1039/C5NJ00787A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C27 H31 Er O11'
_chemical_formula_sum            'C27 H31 Er O11'
_chemical_formula_weight         698.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.425(5)
_cell_length_b                   5.3513(11)
_cell_length_c                   22.945(5)
_cell_measurement_reflns_used    30827
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.504
_cell_measurement_theta_min      1.775
_cell_volume                     2999.0(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.1229
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26496
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.9320
_exptl_absorpt_correction_T_min  0.3290
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         1.774
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.97(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.953
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.999
_reflns_number_gt                4452
_reflns_number_total             6590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00787a2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7055006--7055011.cif.
;
_cod_database_code               7055007
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.330
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.02838 0.97162
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C13-C18
 1.4 with sigma of 0.01
 C5-C6 = C7-C8 = C8-C9
 1.39 with sigma of 0.02
 C5-C6 \\sim C17-C18
 with sigma of 0.02
 C7-C8 \\sim C16-C17
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C3) = Uanis(C2)
Uanis(C21) = Uanis(C20)
Uanis(C23) = Uanis(C27)
Uanis(C17) = Uanis(C15)
Uanis(C19) = Uanis(C1)
Uanis(O8) = Uanis(O7)
Uanis(O1Z) = Uanis(O2Z)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27)
5.c X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6A), O9(H9A)
;
_olex2_submission_special_instructions 'No special instructions were received'