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_7055006
_publ_section_title
;
 Rare earth 3-(4&#x2032;-hydroxyphenyl)propionate complexes
;
_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         'C54 H60 Ce2 O21'
_chemical_formula_sum            'C54 H60 Ce2 O21'
_chemical_formula_weight         1325.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                116.872(5)
_cell_angle_beta                 93.433(5)
_cell_angle_gamma                92.854(5)
_cell_formula_units_Z            2
_cell_length_a                   14.2020(11)
_cell_length_b                   15.9564(14)
_cell_length_c                   16.1020(11)
_cell_measurement_reflns_used    29992
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.268
_cell_measurement_theta_min      1.424
_cell_volume                     3236.9(5)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.1299
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20909
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.424
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   0.9643
_exptl_transmission_factor_min   0.7581
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         11352
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.000
_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          0.1755
_refine_ls_wR_factor_ref         0.1891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7369
_reflns_number_total             11352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00787a2.cif
_cod_data_source_block           compound2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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               7055006
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. 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
2. Shared sites
{C29, C229}
3. Restrained distances
 C4-C5 = C5-C6 = C6-C7 = C7-C8 = C8-C9 = C9-C4
 1.4 with sigma of 0.02
 C104-C105 = C105-C106 = C106-C107 = C107-C108 = C108-C109 = C109-C104
 1.4 with sigma of 0.02
 C231-C36 = C231-C232 = C232-C233 = C233-C34
 1.4 with sigma of 0.02
 C4-C6 = C5-C7 = C6-C8 = C7-C9 = C8-C4 = C9-C5
 2.38 with sigma of 0.02
 C231-C233 = C231-C35 = C232-C36 = C232-C34
 2.38 with sigma of 0.02
 C230-C36 = C230-C232
 2.55 with sigma of 0.02
 C231-C36 \\sim C231-C232
 with sigma of 0.02
 C230-C36 \\sim C230-C232
 with sigma of 0.02
4. Restrained planarity
 C34, C35, C36, C231, C232, C233, C230, O12
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uiso(C232) = Uiso(C233)
Uiso(C231) = Uiso(C233)
6. Others
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) C103(0.5) H10A(0.5) H10B(0.5) C4(0.5)
 C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9A(0.5)
 C33(0.7) H33(0.7) C32(0.7) H32(0.7) C104(0.5) C109(0.5) H109(0.5) C102(0.5)
 H10C(0.5) H10D(0.5) C3(0.5) H3A(0.5) H3B(0.5) C105(0.5) H105(0.5) C106(0.5)
 H106(0.5) C107(0.5) C108(0.5) H108(0.5) C31(0.7) C30(0.7) H30A(0.7) H30B(0.7)
 C29(0.7) H29A(0.7) H29B(0.7) C233(0.3) H233(0.3) C230(0.3) H23A(0.3) H23B(0.3)
 C232(0.3) H232(0.3) C231(0.3) C229(0.3) H22A(0.3) H22B(0.3)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C103(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B),
 C21(H21A,H21B), C38(H38A,H38B), C39(H39A,H39B), C47(H47A,H47B), C48(H48A,H48B),
  C102(H10C,H10D), C3(H3A,H3B), C30(H30A,H30B), C29(H29A,H29B), C230(H23A,H23B),
  C229(H22A,H22B)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9A), C14(H14), C15(H15), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27), C33(H33), C32(H32), C41(H41), C42(H42),
  C44(H44), C45(H45), C50(H50), C51(H51), C53(H53), C54(H54), C109(H109),
 C105(H105), C106(H106), C108(H108), C35(H35), C233(H233), C232(H232)
7.c X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2), O3Z(H3Z1,H3Z2)
7.d Idealised tetrahedral OH refined as rotating group:
 O6(H6H), O9(H9), O12(H12), O15(H15H), O18(H18H)
;
_olex2_submission_special_instructions 'No special instructions were received'