Correlation between the molecular structure and the kinetics of decomposition of azamacrocyclic copper(ii) complexes.
Acosta-Rueda, Laura; Delgado-Pinar, Estefanía; Pitarch-Jarque, Javier; Rodríguez, Alexis; Blasco, Salvador; González, Jorge; Basallote, Manuel G.; García-España, Enrique; Dalton transactions (Cambridge, England : 2003) 44 (2015) 8255–8266; doi:10.1039/c5dt00408j

data_7034655
_publ_section_title
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 Correlation between the molecular structure and the kinetics of
 decomposition of azamacrocyclic copper(ii) complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8255
_journal_page_last               8266
_journal_paper_doi               10.1039/c5dt00408j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H41 Cu2 N8 O, 3(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C24 H45 Cl3 Cu2 N8 O15'
_chemical_formula_weight         919.11
_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   mixed
_audit_creation_date             2014-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-01-12 deposited with the CCDC.
2015-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.723(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4620(3)
_cell_length_b                   13.5450(4)
_cell_length_c                   16.6510(6)
_cell_measurement_reflns_used    11026
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3590.90(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19921
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.279
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  0.5195
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.3000
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0689P)^2^+5.2384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4841
_reflns_number_total             6292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00408j2.cif
_cod_data_source_block           crystal3
_cod_depositor_comments
'Adding full bibliography for 7034653--7034656.cif.'
_cod_database_code               7034655
_shelxl_version_number           2013-4
_exptl_absorpt_correction_t_ave  0.5163
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups, All
  O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
 H2B-O2
 0.82 with sigma of 0.01
 H2A-O2
 0.82 with sigma of 0.01
 H3BB-O3B
 0.82 with sigma of 0.02
 O3B-H3BA
 0.82 with sigma of 0.02
 H3AB-O3A
 0.82 with sigma of 0.02
 O3A-H3AA
 0.82 with sigma of 0.02
3. Rigid bond restraints
 Cl1, O13A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: O3A(0.5) H3AA(0.5) H3AB(0.5) O3B(0.5) H3BA(0.5) H3BB(0.5)
 O24B(0.5) O22B(0.5) O24A(0.5) O23B(0.5) O14A(0.5) O13A(0.5) O12A(0.5)
 O12B(0.5) O14B(0.5) O22A(0.5) O13B(0.5) O23A(0.5)
5.a Rotating group with stretchable bonds:
 O3A(H3AA,H3AB), O3B(H3BA,H3BB), O2(H2A,H2B), O1(H1)
5.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N8(H8), N6(H6)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C24(H24A,H24B), C13(H13A,H13B),
 C8(H8A,H8B), C23(H23A,H23B), C7(H7A,H7B), C19(H19A,H19B), C1(H1A,H1B),
 C21(H21A,H21B), C20(H20A,H20B)
5.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C16(H16), C3(H3), C4(H4A), C17(H17)
5.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C10(H10A,H10B,H10C)
;