Influence of the chain length and metal : ligand ratio on the self-organization processes of Cu<sup>2+</sup> complexes of [1 + 1] 1H-pyrazole azamacrocycles.
Lopera, Alberto; Gil-Martínez, Ariadna; Pitarch-Jarque, Javier; Verdejo, Begoña; Blasco, Salvador; Clares, M. Paz; Jiménez, Hermas R; García-España, Enrique; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8614–8624; doi:10.1039/d0dt01056a

data_7704617
_publ_section_title
;
 Influence of the chain length and metal&#x2009;:&#x2009;ligand ratio on
 the self-organization processes of Cu<sup>2+</sup> complexes of [1 + 1]
 1H-pyrazole azamacrocycles.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8614
_journal_page_last               8624
_journal_paper_doi               10.1039/d0dt01056a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C24 H46 Cu2 N12, 1.56(Cl), 2.37(H2 O), 0.44(Br)'
_chemical_formula_sum            'C24 H50.74 Br0.44 Cl1.56 Cu2 N12 O2.37'
_chemical_formula_weight         762.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-06-01
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-01 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7810(5)
_cell_length_b                   9.13400(10)
_cell_length_c                   21.3720(6)
_cell_measurement_reflns_used    7617
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3258.02(14)
_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, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13925
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.761
_exptl_absorpt_coefficient_mu    2.012
_exptl_absorpt_correction_T_max  0.3821
_exptl_absorpt_correction_T_min  0.3699
_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_colour_primary    blue
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1590
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.072
_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     451
_refine_ls_number_reflns         7452
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0457
_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          0.1203
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4978
_reflns_number_total             7452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01056a2.cif
_cod_data_source_block           2prime_hexa
_cod_depositor_comments
'Adding full bibliography for 7704616--7704620.cif.'
_cod_database_code               7704617
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.500
_exptl_absorpt_correction_t_ave  0.3769
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2A,H2B} of O2, {H3A,H3B} of O3, All C(H,H) groups, All
  C(H,H,H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  {H1C,H1D} of O1
2. Restrained distances
 H2A-Cl2_$3
 2.75 with sigma of 0.02
 H3A-Br2_$2
 2.53 with sigma of 0.01
 H3B-Br2_$1
 2.42 with sigma of 0.01
 H2B-O3
 2.14 with sigma of 0.02
 O3-H3B = O3-H3A
 0.85 with sigma of 0.01
 H3B-H3A
 1.34 with sigma of 0.04
 N12-C22B \\sim N12-C22A
 with sigma of 0.02
 C9A-C10 \\sim C9B-C10 \\sim C9A-C8A \\sim C9B-C8B
 with sigma of 0.02
 N12-C22A \\sim N11-C20B
 with sigma of 0.02
 C21B-C20B \\sim C21A-C20B \\sim C22B-C21B \\sim C22A-C21A
 with sigma of 0.02
3. Rigid bond restraints
 C22B, C21A, C21B, C20B
 with sigma for 1-2 distances of 0.025 and sigma for 1-3 distances of 0.05
4. Uiso/Uaniso restraints and constraints
Uanis(C22B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21B) = Uanis(C21A)
Uanis(C22A) = Uanis(C22B)
5. Others
 Sof(H5B)=Sof(H10C)=Sof(H10D)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=
 Sof(H9BB)=1-FVAR(1)
 Sof(H5A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H10A)=
 Sof(H10B)=FVAR(1)
 Sof(Br1)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
 Sof(Br2)=1-FVAR(3)
 Sof(Cl2)=FVAR(3)
 Sof(H12A)=Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(4)
 Sof(H12)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C22B)=Sof(H22C)=Sof(H22D)=
 Sof(C20A)=Sof(H20C)=Sof(H20D)=FVAR(4)
 Sof(O3)=Sof(H3A)=Sof(H3B)=FVAR(5)
 Sof(O2)=Sof(H2A)=Sof(H2B)=FVAR(6)
 Fixed X: H3B(0.284169) H2A(0.29831) H2B(0.30458)
 Fixed Y: H3B(0.577129) H2A(0.26912) H2B(0.4158)
 Fixed Z: H3B(-0.020881) H2A(0.05547) H2B(0.05415)
6.a Free rotating group:
 O1(H1C,H1D)
6.b Ternary CH refined with riding coordinates:
 N10(H10), N4(H4), N1(H1), N7(H7), N6(H6), N5(H5A), N5(H5B), N11(H11),
 N12(H12A), N12(H12)
6.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C17(H17A,H17B), C23(H23A,H23B), C5(H5C,H5D), C19(H19A,H19B),
 C6(H6A,H6B), C13(H13A,H13B), C1(H1A,H1B), C11(H11A,H11B), C18(H18A,H18B),
 C12(H12B,H12C), C24(H24A,H24B), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10(H10A,H10B),
  C10(H10C,H10D), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C20B(H20A,H20B), C22A(H22A,
 H22B), C21B(H21A,H21B), C21A(H21C,H21D), C22B(H22C,H22D), C20A(H20C,H20D)
6.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3)
;
_shelx_res_checksum              8417
_olex2_submission_special_instructions 'No special instructions were received'