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_7055011
_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         'C64 H69 Na Nd2 O23, H2 O, 3(C H4 O)'
_chemical_formula_sum            'C67 H83 Na Nd2 O27'
_chemical_formula_weight         1631.80
_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             2015-05-22
_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                78.16(3)
_cell_angle_beta                 70.63(3)
_cell_angle_gamma                86.33(3)
_cell_formula_units_Z            2
_cell_length_a                   15.328(3)
_cell_length_b                   15.480(3)
_cell_length_c                   16.300(3)
_cell_measurement_reflns_used    43827
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.046
_cell_measurement_theta_min      1.344
_cell_volume                     3571.0(14)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1163
_diffrn_reflns_av_unetI/netI     0.1473
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31950
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.344
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.9277
_exptl_transmission_factor_min   0.7018
_refine_diff_density_max         2.174
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         12470
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.002
_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          0.1616
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7672
_reflns_number_total             12470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00787a2.cif
_cod_data_source_block           compound4.cif
_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               7055011
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.702
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, {H14H,H2ZD,H4Z} of C4Z, All C(H) groups, All C(H,H) groups,
   All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  {H4Z1,H4Z2,H4Z3} of C4Z, {H6ZA,H6ZB,H6ZC} of C6Z, {H2ZA,H2ZB,H2ZC} of C2Z,
  {H5ZA,H5ZB,H5ZC} of C5Z
2. Restrained distances
 C22-C23 = C23-C24 = C24-C25 = C25-C26 = C26-C27 = C27-C22
 1.4 with sigma of 0.02
 C16-C17 = C13-C18
 1.4 with sigma of 0.02
 O2Z-H2ZD = O12-H14H
 0.9 with sigma of 0.02
 O9-H9H = O4Z-H4Z = O18-H18H = O3Z-H3ZA = O3Z-H3ZB
 0.92 with sigma of 0.02
 C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C18 = C18-C13
 1.4 with sigma of 0.02
 Na1-H2ZD
 2.39 with sigma of 0.02
3. Rigid bond restraints
 C13, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C47, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim O9:
within 1.7A with sigma of 0.05 and sigma for terminal atoms of 0.01
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A
with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(O4Z) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, : with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(C28)
Uiso(C4Z) = Uiso(C6Z)
Uanis(O4Z) = Uanis(O5Z)
Uanis(O7) = Uanis(O8)
Uanis(C37) = Uanis(C38)
Uanis(O5) = Uanis(O10)
Uanis(C4) = Uanis(C5)
Uanis(C21) = Uanis(C20)
Uanis(O9) = Uanis(O21)
Uiso(H3ZA) = Uiso(H1Z1)
Uiso(H4Z) = Uiso(H5ZD)
Uanis(C14) = Uanis(C12)
Uanis(C13) = Uanis(C12)
Uanis(C16) = Uanis(C15)
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), C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B),
  C47(H47A,H47B), C48(H48A,H48B), C56(H56A,H56B), C57(H57A,H57B)
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), C32(H32), C33(H33), C35(H35), C36(H36),
  C41(H41), C42(H42), C44(H44), C45(H45), C50(H50), C51(H51), C53(H53),
 C54(H54), C59(H59), C60(H60), C62(H62), C63(H63)
5.c X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2)
5.d Idealised Me refined as rotating group:
 C2Z(H2ZA,H2ZB,H2ZC), C5Z(H5ZA,H5ZB,H5ZC), C6Z(H6ZA,H6ZB,H6ZC), C4Z(H4Z1,H4Z2,
 H4Z3)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3H), O5Z(H5ZD), O6(H6H), O6Z(H6ZD), O9(H9H), O15(H15H), O21(H21)
;
_olex2_submission_special_instructions 'No special instructions were received'