Metallamacrocycle formation through dimerization of metal bioconjugates derived from amino acids and peptides.
Álvarez, Celedonio M; García-Rodríguez, Raúl; Miguel, Daniel; Dalton transactions (Cambridge, England : 2003) 45 (2016) 963–972; doi:10.1039/c5dt01256b

data_7037354
_publ_section_title
;
 Metallamacrocycle formation through dimerization of metal bioconjugates
 derived from amino acids and peptides.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              963
_journal_page_last               972
_journal_paper_doi               10.1039/c5dt01256b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C12 H9 N2 O5 Re), C4 H8 O'
_chemical_formula_sum            'C28 H26 N4 O11 Re2'
_chemical_formula_weight         966.93
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.703(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.490(4)
_cell_length_b                   15.058(4)
_cell_length_c                   16.017(4)
_cell_measurement_reflns_used    572
_cell_measurement_temperature    296
_cell_measurement_theta_max      16.62
_cell_measurement_theta_min      2.55
_cell_volume                     3207.0(15)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.719
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1611
_diffrn_reflns_av_unetI/netI     0.2587
_diffrn_reflns_laue_measured_fraction_full 0.719
_diffrn_reflns_laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8212
_diffrn_reflns_point_group_measured_fraction_full 0.719
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         23.261
_diffrn_reflns_theta_min         1.828
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.604
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.196211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0680 before and 0.0401 after correction.
The Ratio of minimum to maximum transmission is 0.1962.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.2069
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0617P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1848
_reflns_number_total             4532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01256b2.cif
_cod_data_source_block           C_2b_rg109am
_cod_depositor_comments
'Adding full bibliography for 7037352--7037358.cif.'
_cod_original_cell_volume        3207.3(15)
_cod_database_code               7037354
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 O9, C46, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C12, Re1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C20(H20A,H20B), C23(H23A,H23B), C26(H26A,H26B), C39(H39A,
 H39B), C40(H40A,H40B), C44(H44A,H44B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C25(H25), C29(H29), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C41(H41)
;
_shelx_res_checksum              85849
_olex2_submission_special_instructions 'No special instructions were received'