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_7228053
_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         'C15 H15 N O8 Yb'
_chemical_formula_sum            'C15 H15 N O8 Yb'
_chemical_formula_weight         510.32
_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             2017-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-09 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                63.350(2)
_cell_angle_beta                 71.042(2)
_cell_angle_gamma                82.5615(19)
_cell_formula_units_Z            2
_cell_length_a                   8.5054(2)
_cell_length_b                   10.2435(2)
_cell_length_c                   10.9144(3)
_cell_measurement_reflns_used    12740
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5724
_cell_measurement_theta_min      3.3329
_cell_volume                     803.65(4)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40)'
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40)'
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40)'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 25.00 88.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 38.0000 -150.0000 63 #__ type_ start__ end____ width___ exp.time_ 2 omega -3.00 82.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 55.0000 147.0000 85 #__ type_ start__ end____ width___ exp.time_ 3 omega -18.00 92.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 77.0000 -60.0000 110 #__ type_ start__ end____ width___ exp.time_ 4 omega -59.00 44.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 -55.0000 -175.0000 103 #__ type_ start__ end____ width___ exp.time_ 5 omega -30.00 40.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 -38.0000 0.0000 70 #__ type_ start__ end____ width___ exp.time_ 6 omega 34.00 76.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 179.0000 30.0000 42 #__ type_ start__ end____ width___ exp.time_ 7 omega 5.00 85.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 38.0000 90.0000 80 #__ type_ start__ end____ width___ exp.time_ 8 omega 34.00 88.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 14.4190 179.0000 -150.0000 54 #__ type_ start__ end____ width___ exp.time_ 9 omega -91.00 -52.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -15.2002 153.0000 -126.0000 39 #__ type_ start__ end____ width___ exp.time_ 10 omega -93.00 -67.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -15.2002 155.0000 49.0000 26'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0782193000
_diffrn_orient_matrix_UB_12      0.0226442000
_diffrn_orient_matrix_UB_13      -0.0120262000
_diffrn_orient_matrix_UB_21      0.0334940000
_diffrn_orient_matrix_UB_22      0.0711519000
_diffrn_orient_matrix_UB_23      -0.0488486000
_diffrn_orient_matrix_UB_31      0.0231951000
_diffrn_orient_matrix_UB_32      -0.0207162000
_diffrn_orient_matrix_UB_33      -0.0572991000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15243
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         30.641
_diffrn_reflns_theta_min         3.340
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) 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    2.109
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4490
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0127P)^2^+0.6471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4402
_reflns_number_total             4490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00481h2.cif
_cod_data_source_block           mb3
_cod_depositor_comments
'Adding full bibliography for 7228053--7228056.cif.'
_cod_database_code               7228053
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H20 N2 O2 Yb'
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 0
_reflns_odcompleteness_theta     28.02
_olex2_refinement_description
;
The hydrogens on the coordinated water (O501) were located in 
a difference map.
They were allowed to refine with a distance restraint (DFIX 0.85) 
and thermal parameters equal to 1.5 times that of O501 to which 
they were attached.

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. Restrained distances
 O501-H50A = O501-H50B
 0.85 with sigma of 0.008
3.a Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C204(H204), C205(H205), C304(H304), C305(H305),
 C402(H402)
3.b Idealised Me refined as rotating group:
 C404(H40A,H40B,H40C), C405(H40D,H40E,H40F)
;
_shelx_res_checksum              71286
_olex2_submission_special_instructions 'No special instructions were received'