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_7055008
_publ_section_title
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 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         'C108 H120 La4 O42, 4(H2 O), C H4 O'
_chemical_formula_sum            'C109 H132 La4 O47'
_chemical_formula_weight         2749.78
_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             2015-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
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2015-07-13 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                89.014(2)
_cell_angle_beta                 78.289(2)
_cell_angle_gamma                64.668(3)
_cell_formula_units_Z            2
_cell_length_a                   15.2502(9)
_cell_length_b                   16.6406(10)
_cell_length_c                   25.6709(14)
_cell_measurement_reflns_used    87057
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      30.086
_cell_measurement_theta_min      0.813
_cell_volume                     5747.7(6)
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_laue_measured_fraction_full 0.982
_diffrn_reflns_laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80774
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         0.813
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   0.9624
_exptl_transmission_factor_min   0.7473
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1500
_refine_ls_number_reflns         25932
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0814
_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          0.1419
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20184
_reflns_number_total             25932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00787a2.cif
_cod_data_source_block           compound1.cif
_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               7055008
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6H of O6, H9H of O9, H12H of O12, H18H of O18, H11Z of
  O11Z, H3H of O3, H36H of O36, H33H of O33, H30H of O30, H27H of O27, H24H of
  O24, H21H of O21, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H15H of O15
2. Restrained distances
 O10Z-H101 = O10Z-H100 = O8Z-H80A = O8Z-H80B
 0.9 with sigma of 0.02
3.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), C65(H65A,H65B), C66(H66A,
 H66B), C74(H74A,H74B), C75(H75A,H75B), C83(H83A,H83B), C84(H84A,H84B),
 C92(H92A,H92B), C93(H93A,H93B), C101(H10A,H10B), C102(H10C,H10D), C57(H57A,
 H57B)
3.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), C68(H68), C69(H69), C71(H71),
  C72(H72), C77(H77), C78(H78), C80(H80), C81(H81), C86(H86), C87(H87),
 C89(H89), C90(H90), C95(H95), C96(H96), C98(H98), C99(H99), C104(H104),
 C105(H105), C107(H107), C108(H108)
3.c Tetrahedral OH refined with riding coordinates:
 O15(H15H)
3.d X=CH2 refined with riding coordinates:
 O1Z(H1Z1,H1Z2), O2Z(H2Z1,H2Z2), O3Z(H3Z1,H3Z2), O4Z(H4Z1,H4Z2), O5Z(H5Z1,H5Z2)
3.e Idealised Me refined as rotating group:
 C1Z(H1Z3,H1Z4,H1Z5)
3.f Idealised tetrahedral OH refined as rotating group:
 O3(H3H), O12(H12H), O18(H18H), O21(H21H), O24(H24H), O27(H27H), O33(H33H),
 O36(H36H), O11Z(H11Z)
;
_olex2_submission_special_instructions 'No special instructions were received'