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_7055010
_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         'C63 H67 Ce2 Na O23, 3(H2 O)'
_chemical_formula_sum            'C63 H73 Ce2 Na O26'
_chemical_formula_weight         1549.44
_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                103.726(2)
_cell_angle_beta                 107.053(2)
_cell_angle_gamma                94.662(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0063(7)
_cell_length_b                   15.3267(7)
_cell_length_c                   16.4093(7)
_cell_measurement_reflns_used    40363
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.190
_cell_measurement_theta_min      1.350
_cell_volume                     3458.6(3)
_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    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.1414
_diffrn_reflns_av_unetI/netI     0.2013
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29745
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.350
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         6.454
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.397
_refine_ls_extinction_coef       13241(92)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         11923
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.1257
_refine_ls_shift/su_max          0.036
_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          0.3033
_refine_ls_wR_factor_ref         0.3247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9547
_reflns_number_total             11923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00787a2.cif
_cod_data_source_block           compound2b
_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               7055010
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.819
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 18.82316 -17.82316
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H15H of O15, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  H3 of O3
3. Restrained distances
 C31-C32 = C32-C33 = C33-C34 = C34-C35 = C35-C36 = C36-C31
 1.39 with sigma of 0.02
 C40-C41 = C44-C45
 1.4 with sigma of 0.02
 C43-C44 = C45-C40
 1.39 with sigma of 0.02
 C58-C59 = C60-C61 = C62-C63
 1.39 with sigma of 0.02
 C59-C60 = C61-C62 = C63-C58
 1.39 with sigma of 0.02
 C52-C53 = C53-C54
 1.4 with sigma of 0.02
 C49-C50
 1.39 with sigma of 0.02
 C47-C48 = C46-C47 = C48-C49
 1.4 with sigma of 0.002
 C41-C42 = C42-C43 = C39-C40
 1.4 with sigma of 0.002
 C49-C54
 1.4 with sigma of 0.002
 C29-C30
 1.57 with sigma of 0.02
 C31-C33 = C32-C34 = C33-C35 = C34-C36 = C35-C31 = C36-C32
 2.39 with sigma of 0.02
4. Restrained planarity
 C40, C41, C42, C43, C44, C45
 with sigma of 0.1
5. Rigid bond restraints
 C30, C31
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C46, C47
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C56, C57
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C61, C62
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C7, C8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C24, C25
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C34, C35
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C47, C48
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C60, C61
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O20, C55
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C11, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C16, C17
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C22, C23
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C13, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C62, C63
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C29, C30
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A
with sigma of 0.05 and sigma for terminal atoms of 0.01
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 1.7A with sigma
of 0.05 and sigma for terminal atoms of 0.01
C47 \\sim C48 \\sim C49 \\sim C52 \\sim C53: within 1.7A with sigma of 0.05 and
sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C63) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) = Uanis(C39)
Uanis(C50) = Uanis(C51)
Uanis(C57) = Uanis(C56)
Uanis(C30) = Uanis(C29)
Uanis(C34) = Uanis(C33)
Uanis(C58) = Uanis(C59)
Uanis(C55) = Uanis(O19)
7. Others
 Fixed k1: basf(-17.82316)
8.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), C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B),
  C47(H47A,H47B), C48(H48A,H48B), C56(H56A,H56B), C57(H57A,H57B)
8.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), C41(H41), C42(H42), C44(H44), C45(H45),
  C50(H50), C51(H51), C53(H53), C54(H54), C59(H59), C60(H60), C62(H62),
 C63(H63), C33(H33), C35(H35), C36(H36)
8.c Tetrahedral OH refined with riding coordinates:
 O3(H3)
8.d X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2)
8.e Idealised tetrahedral OH refined as rotating group:
 O15(H15H)
;
_olex2_submission_special_instructions 'No special instructions were received'