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_7034656
_publ_section_title
;
 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 H40 Cu N8, 2(Cl O4)'
_chemical_formula_sum            'C24 H40 Cl2 Cu N8 O8'
_chemical_formula_weight         703.08
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-01-25 deposited with the CCDC.
2015-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7470(2)
_cell_length_b                   14.2670(3)
_cell_length_c                   20.3170(4)
_cell_measurement_reflns_used    6563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_cell_volume                     3106.36(11)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10616
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.525
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         5456
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0939P)^2^+2.0898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4144
_reflns_number_total             5456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00408j2.cif
_cod_data_source_block           crystal4
_cod_depositor_comments
'Adding full bibliography for 7034653--7034656.cif.'
_cod_database_code               7034656
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10A,H10B,H10C} of C10, All C(H,H) groups, All C(H,H,H,H)
  groups, All N(H) groups
 At 1.5 times of:
  {H22D,H22E,H22F} of C22B, {H22A,H22B,H22C} of C22A
2. Rigid bond restraints
 O21B, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O23B, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, O14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, O14B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N7A, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O23A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O22A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim N8: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01
C12 \\sim N4 \\sim C11: within 1.7A with sigma of 0.008 and sigma for terminal
atoms of 0.01
C7 \\sim N2 \\sim C6: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
N7B \\sim N7A \\sim C21 \\sim C20 \\sim N6: within 1.7A with sigma of 0.008 and
sigma for terminal atoms of 0.01
Uanis(O14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H24C(0.7) H24D(0.7) H24A(0.3) H24B(0.3) O14B(0.75) O13A(0.75)
 O11A(0.75) O12A(0.75) O22A(0.5) O21A(0.5) O23A(0.5) O23B(0.5) O21B(0.5)
 O22B(0.5) N7A(0.7) H21C(0.7) H21D(0.7) H21A(0.3) H21B(0.3) C23A(0.7) H23A(0.7)
 H23B(0.7) C22A(0.7) H22A(0.7) H22B(0.7) H22C(0.7) N7B(0.3) C23B(0.3) H23C(0.3)
 H23D(0.3) C22B(0.3) H22D(0.3) H22E(0.3) H22F(0.3) O11B(0.25) O12B(0.25)
 O14A(0.25) O13B(0.25)
5.a Riding coordinates:
 C1(H1A,H1B), C9(H9A,H9B), C7(H7A,H7B), C8(H8A,H8B), C5(H5), C13(H13A,H13B),
 C12(H12A,H12B), N6(H6), C10(H10A,H10B,H10C), C3(H3), C11(H11A,H11B), C19(H19A,
 H19B), C17(H17), C16(H16), C4(H4A), C15(H15), C20(H20A,H20B)
5.b Ternary CH refined with riding coordinates:
 N8(H8), N2(H2), N4(H4)
5.c Secondary CH2 refined with riding coordinates:
 C24(H24C,H24D), C24(H24A,H24B), C21(H21C,H21D), C21(H21A,H21B), C23A(H23A,
 H23B), C23B(H23C,H23D)
5.d Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
;