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_7037356
_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         'C26 H20 Mn2 N6 O12, C H4 O'
_chemical_formula_sum            'C27 H24 Mn2 N6 O13'
_chemical_formula_weight         750.40
_chemical_name_systematic
;
 ?
;
_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             2015-08-18
_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                 94.052(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.307(10)
_cell_length_b                   11.341(9)
_cell_length_c                   24.874(19)
_cell_measurement_reflns_used    621
_cell_measurement_temperature    296
_cell_measurement_theta_max      18.034
_cell_measurement_theta_min      2.415
_cell_volume                     3463(5)
_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 0.727
_diffrn_measured_fraction_theta_max 0.981
_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  0.2356
_diffrn_reflns_av_unetI/netI     0.2590
_diffrn_reflns_laue_measured_fraction_full 0.727
_diffrn_reflns_laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14362
_diffrn_reflns_point_group_measured_fraction_full 0.727
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         23.349
_diffrn_reflns_theta_min         1.641
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.193874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0987 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.0939.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.2075
_refine_ls_R_factor_gt           0.0775
_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^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1891
_reflns_number_total             4945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01256b2.cif
_cod_data_source_block           C_4a_rg174bm
_cod_depositor_comments
'Adding full bibliography for 7037352--7037358.cif.'
_cod_database_code               7037356
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C27(H27A,H27B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26)
2.c Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C)
2.d Idealised tetrahedral OH refined as rotating group:
 O90(H90)
;
_shelx_res_checksum              59740
_olex2_submission_special_instructions 'No special instructions were received'