A designed and potentially decadentate ligand for use in lanthanide(iii) catalysed biomass transformations: targeting diastereoselective trans-4,5-diaminocyclopentenone derivatives.
Peewasan, Krisana; Merkel, Marcel P.; Fuhr, Olaf; Powell, Annie K.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2331–2336; doi:10.1039/d0dt00183j

data_7703355
_publ_section_title
;
 A designed and potentially decadentate ligand for use in lanthanide(iii)
 catalysed biomass transformations: targeting diastereoselective
 trans-4,5-diaminocyclopentenone derivatives.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2331
_journal_page_last               2336
_journal_paper_doi               10.1039/d0dt00183j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C34 H36 Br2 Er N11 O6, 2(N O3)'
_chemical_formula_sum            'C34 H36 Br2 Er N13 O12'
_chemical_formula_weight         1145.84
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-21 deposited with the CCDC.	2020-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.752(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4509(3)
_cell_length_b                   18.1610(4)
_cell_length_c                   21.2663(6)
_cell_measurement_reflns_used    8534
_cell_measurement_temperature    180
_cell_measurement_theta_max      64.26
_cell_measurement_theta_min      20.55
_cell_volume                     4798.4(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_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      180
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29620
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.496
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    7.403
_exptl_absorpt_correction_T_max  0.4326
_exptl_absorpt_correction_T_min  0.0267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       needle
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         11293
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0534
_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^)+(0.1090P)^2^+3.3376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9099
_reflns_number_total             11293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00183j2.cif
_cod_data_source_block           kp269
_cod_depositor_comments
'Adding full bibliography for 7703352--7703355.cif.'
_cod_database_code               7703355
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.319
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O13-O15
 2.11 with sigma of 0.02
 O15-N14 = O14-N14 = O13-N14
 1.22 with sigma of 0.02
3. Restrained planarity
 N14, O13, O14, O15
 with sigma of 0.1
4. Others
 Fixed Sof: O10(0.5) O12(0.5) N13(0.5) N14(0.5) O14(0.5) O15(0.5) O13(0.5)
5.a Rotating group:
 O6(H6A,H6B)
5.b Ternary CH refined with riding coordinates:
 N5(H5), N6(H6)
5.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N8(H8), N10(H10), C3(H3A), C4(H4), C5(H5A), C6(H6C), C8(H8A),
 C12(H12), C14(H14), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33),
  C34(H34)
5.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              71507
_shelx_fab_checksum              73896
_olex2_submission_special_instructions 'No special instructions were received'