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_7704618
_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
'C14 H28.07 Br0.27 Cl0.23 Cu2 N6 O1.07, 1.46(Cl O4)'
_chemical_formula_sum            'C14 H28.07 Br0.27 Cl1.69 Cu2 N6 O6.93'
_chemical_formula_weight         600.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.1587(5)
_cell_length_b                   22.0003(10)
_cell_length_c                   17.5957(7)
_cell_measurement_reflns_used    7431
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      31.6260
_cell_measurement_theta_min      3.5090
_cell_volume                     4319.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_details
;
  1 omega  -31.00    2.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -38.0000  120.0000 33

  2 omega  -53.00    7.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -77.0000   90.0000 60

  3 omega   63.00  103.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7590 -178.0000 -120.0000 40

  4 omega    1.00   99.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7590   38.0000   90.0000 98
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23582
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.525
_diffrn_reflns_theta_min         2.948
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2446
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         7246
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0424P)^2^+5.8122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5551
_reflns_number_total             7246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01056a2.cif
_cod_data_source_block           3_4cu
_cod_depositor_comments
'Adding full bibliography for 7704616--7704620.cif.'
_cod_database_code               7704618
_shelx_shelxl_version_number     2018/3
_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 O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(Cl3)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Sof(O3)=Sof(H3B)=1-FVAR(2)
 Sof(Cl2)=Sof(O21)=Sof(O23)=0.5*FVAR(3)
 Sof(O22)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 N6(H6), N4(H4), N5(H5), N3(H3A)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C7(H7A,H7B), C5(H5A,H5B), C1(H1A,H1B),
 C14(H14A,H14B), C6(H6A,H6B), C11(H11A,H11B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
4.d Tetrahedral OH refined with riding coordinates:
 O3(H3B)
;
_shelx_res_checksum              16449
_olex2_submission_special_instructions 'No special instructions were received'