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_7037353
_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         'C24 H18 Mn2 N4 O10, 2(C6 H16 N), 2(Cl O4)'
_chemical_formula_sum            'C36 H50 Cl2 Mn2 N6 O18'
_chemical_formula_weight         1035.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.104(4)
_cell_length_b                   28.519(9)
_cell_length_c                   13.023(4)
_cell_measurement_reflns_used    965
_cell_measurement_temperature    296
_cell_measurement_theta_max      21.388
_cell_measurement_theta_min      2.316
_cell_volume                     4867(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21430
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.378
_diffrn_reflns_theta_max         23.378
_diffrn_reflns_theta_min         1.428
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.666080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1343P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.2059
_reflns_Friedel_coverage         0.903
_reflns_friedel_fraction_full    0.996
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                3553
_reflns_number_total             5631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01256b2.cif
_cod_data_source_block           C_2a1_rg52bm
_cod_depositor_comments
'Adding full bibliography for 7037352--7037358.cif.'
_cod_database_code               7037353
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.05(7) -0.05(7)
2. 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 C(H,H,H,H,H,H) groups
3. Restrained distances
 N80-C85A = N80-C85B
 1.478 with sigma of 0.005
 C85A-C86 = C85B-C86
 1.505 with sigma of 0.005
 N80-C86
 2.488 with sigma of 0.005
4. Rigid bond restraints
 O11, O12, O13, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O21, O22, O23, O24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C81, C82, C83, C84, C85A, C85B, C86
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C71, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O11 \\sim O12 \\sim O13 \\sim O14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
O21 \\sim O22 \\sim O23 \\sim O24: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85A \\sim C85B \\sim C86: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85A) \\sim Ueq, Uanis(C85B) \\sim Ueq, Uanis(C86) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
6. Others
 Fixed Sof: C85A(0.7) H85A(0.7) H85B(0.7) C85B(0.3) H85C(0.3) H85D(0.3)
 H86D(0.7) H86E(0.7) H86F(0.7) H86A(0.3) H86B(0.3) H86C(0.3)
7.a Free rotating group:
 N70(H70,C71,H71A,H71B,C72,H72A,H72B,H72C,C73,H73A,H73B,C74,H74A,H74B,H74C,C75,
 H75A,H75B,C76,H76A,H76B,H76C), N80(H80,C81,H81A,H81B,C82,H82A,H82B,H82C,C83,
 H83A,H83B,C84,H84A,H84B,H84C,C85A,H85A,H85B,C85B,H85C,H85D,C86,H86D,H86E,H86F,
 H86A,H86B,H86C)
7.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C27(H27A,H27B), C28(H28A,H28B)
7.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26)
;
_shelx_res_checksum              94650
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'