Structural variety in ytterbium dicarboxylate frameworks and in situ study diffraction of their solvothermal crystallisation
Breeze, Matthew I.; Chamberlain, Thomas W.; Clarkson, Guy J.; de Camargo, Raíssa Pires; Wu, Yue; de Lima, Juliana Fonseca; Millange, Franck; Serra, Osvaldo A.; O'Hare, Dermot; Walton, Richard I.; CrystEngComm 19 (2017) 2424–; doi:10.1039/C7CE00481H

data_7228056
_publ_section_title
;
 Structural variety in ytterbium dicarboxylate frameworks and in situ
 study diffraction of their solvothermal crystallisation
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2424
_journal_paper_doi               10.1039/C7CE00481H
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C18 H13 O8 Yb, C3 H7 N O'
_chemical_formula_sum            'C21 H20 N O9 Yb'
_chemical_formula_weight         603.42
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-03-09 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                110.453(2)
_cell_angle_beta                 102.132(2)
_cell_angle_gamma                109.619(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4515(2)
_cell_length_b                   12.3972(4)
_cell_length_c                   12.5680(3)
_cell_measurement_reflns_used    13197
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3520
_cell_measurement_theta_min      3.0980
_cell_volume                     1079.20(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -58.00 43.00 1.00 25.00 -- 16.32 -57.00 -60.00 101 2 \w -56.00 32.00 1.00 25.00 -- 16.32 -57.00 60.00 88 3 \w -47.00 50.00 1.00 25.00 -- -17.25 57.00-180.00 97 4 \w -91.00 12.00 1.00 25.00 -- -17.25 -57.00 30.00 103 5 \w -79.00 9.00 1.00 25.00 -- -17.25 -38.00-120.00 88 6 \w -90.00 16.00 1.00 25.00 -- -17.25 -77.00-180.00 106 7 \w -91.00 -34.00 1.00 25.00 -- -17.25 150.00-157.74 57 8 \w -80.00 -34.00 1.00 25.00 -- -17.25 133.00 -7.67 46'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0588476000
_diffrn_orient_matrix_UB_12      -0.0601649000
_diffrn_orient_matrix_UB_13      -0.0063111000
_diffrn_orient_matrix_UB_21      -0.0552321000
_diffrn_orient_matrix_UB_22      0.0272633000
_diffrn_orient_matrix_UB_23      0.0219347000
_diffrn_orient_matrix_UB_31      -0.0518766000
_diffrn_orient_matrix_UB_32      -0.0171615000
_diffrn_orient_matrix_UB_33      -0.0607112000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20934
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.595
_diffrn_reflns_theta_min         3.099
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.386
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.105
_refine_diff_density_max         2.462
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0711P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5870
_reflns_number_total             6549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00481h2.cif
_cod_data_source_block           mb5
_cod_depositor_comments
'Adding full bibliography for 7228053--7228056.cif.'
_cod_original_cell_volume        1079.19(6)
_cod_database_code               7228056
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C20 H20 N2 O18P Ir'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_refinement_description
;
All the crystals examined were twinned. The data was collected on the best crystal. 
A suitable twin refinement could not be realized so the refinement was conducted on 
the major twin component and is the data presented here.
The hydrogens on the water were located in a difference map but placed at calculated 
positions for the refinement.
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O1D(H1DA,H1DB), O1E(H1EA,H1EB)
2.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C7A(H7A), C4B(H4B), C5B(H5B), C7B(H7B), C4C(H4C),
 C5C(H5C), C7C(H7C), C101(H101)
2.c Idealised Me refined as rotating group:
 C103(H10A,H10B,H10C), C104(H10D,H10E,H10F)
;
_shelx_res_checksum              68478
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
'Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling'
_oxdiff_exptl_absorpt_empirical_full_max 1.476
_oxdiff_exptl_absorpt_empirical_full_min 0.724
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3
_twin_special_details
'Component 2 rotated by 2.1977\% around [-0.69 0.47 -0.55] (reciprocal) or [-0.90 -0.14 -0.42] (direct) Component 3 rotated by 4.2318\% around [-0.67 -0.59 -0.46] (reciprocal) or [-0.77 -0.49 -0.40] (direct)'