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_7228054
_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         'C9 H5 O6 Yb'
_chemical_formula_sum            'C9 H5 O6 Yb'
_chemical_formula_weight         382.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 95.2274(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.56825(17)
_cell_length_b                   12.66272(19)
_cell_length_c                   6.62290(13)
_cell_measurement_reflns_used    5305
_cell_measurement_temperature    296(3)
_cell_measurement_theta_max      77.5500
_cell_measurement_theta_min      4.1790
_cell_volume                     882.61(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1350213000
_diffrn_orient_matrix_UB_12      -0.0382177000
_diffrn_orient_matrix_UB_13      0.0725536000
_diffrn_orient_matrix_UB_21      0.0491870000
_diffrn_orient_matrix_UB_22      0.1142940000
_diffrn_orient_matrix_UB_23      -0.0079085000
_diffrn_orient_matrix_UB_31      -0.0282293000
_diffrn_orient_matrix_UB_32      0.0165419000
_diffrn_orient_matrix_UB_33      0.2218477000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.644
_diffrn_reflns_theta_min         4.201
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. 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    2.876
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.993
_refine_diff_density_min         -1.777
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2625
_reflns_number_total             3200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00481h2.cif
_cod_data_source_block           rc1_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7228053--7228056.cif.'
_cod_database_code               7228054
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H20 N2 O2 Yb'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
All the samples of the blocks investigated were twinned to some extent making 
the diffraction from the small crystals very weak.
The most promising sample with the least amount of twinning was recorded and 
the structural refinement appears here.

The asymmetric unit contains a terephthalate, a Yb and a formate. Four times 
all this in the unit cell.

Matrices relating the two twin components were
1  1.0000  0.0000  0.0000  0.0000  1.0000  0.0000  0.0000  0.0000  1.0000
2 -1.0000  0.0007 -0.2907 -0.0007 -1.0001 -0.0003  0.0004 -0.0002  1.0001

The volume of the two domains in the crystal from the integration is
  _diffrn_oxdiff_twin_id
  _diffrn_oxdiff_twin_ratio
  _diffrn_oxdiff_twin_reflns_isolated
  _diffrn_oxdiff_twin_reflns_overlapped
 1 0.6644 4033 4763
 2 0.3356 4027 4763

Twinned data refinement with Shelxl/Olex2 from the refinement of the BASF 
on F2 (see Shelx manual for details)
The refined scale factors (twin ratios) were   0.7145(18) 0.2855(18)

1. Twinned data refinement
 Scales: 0.7145(18)
 0.2855(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C12(H12)
;
_shelx_res_checksum              59528
_olex2_submission_special_instructions 'No special instructions were received'