Temperature-dependent 3D structures of lanthanide coordination polymers based on dicarboxylate mixed ligands
Chainok, Kittipong; Ponjan, Nutcha; Theppitak, Chatphorn; Khemthong, Phailyn; Kielar, Filip; Dungkaew, Winya; Zhou, Yan; Batten, Stuart R.; CrystEngComm 20 (2018) 7446–; doi:10.1039/C8CE01430B

data_7231577
_publ_section_title
;
 Temperature-dependent 3D structures of lanthanide coordination polymers
 based on dicarboxylate mixed ligands
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              7446
_journal_paper_doi               10.1039/C8CE01430B
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H16 Er2 O16, 2(H2 O)'
_chemical_formula_sum            'C16 H20 Er2 O18'
_chemical_formula_weight         834.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.0475(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9118(2)
_cell_length_b                   12.3451(3)
_cell_length_c                   10.3400(2)
_cell_measurement_reflns_used    9665
_cell_measurement_temperature    296
_cell_measurement_theta_max      30.521
_cell_measurement_theta_min      3.190
_cell_volume                     1108.21(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34355
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.539
_diffrn_reflns_theta_min         3.190
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.613
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0799 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.8445. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light pink'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 2857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0326
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6323
_reflns_number_total             6761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01430b2.cif
_cod_data_source_block           6er
_cod_depositor_comments
'Adding full bibliography for 7231570--7231583.cif.'
_cod_database_code               7231577
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.581
_shelx_estimated_absorpt_t_min   0.376
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O14-H14A = O16-H16A
 0.84 with sigma of 0.01
 O14-H14B
 0.84 with sigma of 0.01
 H14A-H14B
 1.37 with sigma of 0.02
 O17-H17A
 0.84 with sigma of 0.01
 O16-H16B
 0.84 with sigma of 0.01
 H16A-H16B
 1.355 with sigma of 0.02
 O17-H17B
 0.84 with sigma of 0.01
 H17A-H17B
 1.35 with sigma of 0.02
 O15-H15A
 0.84 with sigma of 0.01
 O15-H15B
 0.84 with sigma of 0.01
 H15B-H15A
 1.37 with sigma of 0.02
 O18-H18A
 0.84 with sigma of 0.01
 O18-H18B
 0.84 with sigma of 0.01
 H18A-H18B
 1.39 with sigma of 0.02
 O13-H13B = O13-H13A
 0.84 with sigma of 0.01
 H13B-H13A
 1.39 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14), C15(H15)
;
_shelx_res_checksum              75612
_olex2_submission_special_instructions 'No special instructions were received'