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_7704616
_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, 4(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C24 H54 Cl4 Cu2 N12 O20'
_chemical_formula_weight         1099.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-27
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-01 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                112.721(6)
_cell_angle_beta                 99.370(5)
_cell_angle_gamma                109.507(5)
_cell_formula_units_Z            1
_cell_length_a                   9.2355(5)
_cell_length_b                   11.6706(7)
_cell_length_c                   11.9460(9)
_cell_measurement_reflns_used    4132
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      1
_cell_volume                     1054.57(15)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.851
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8268
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.898
_diffrn_reflns_theta_min         3.041
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4730
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.6115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4029
_reflns_number_total             4730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01056a2.cif
_cod_data_source_block           1_penta
_cod_depositor_comments
'Adding full bibliography for 7704616--7704620.cif.'
_cod_original_cell_volume        1054.56(13)
_cod_database_code               7704616
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2C,H2D} of O2, All C(H,H) groups, All N(H) groups, All
  N(H,H) groups
 At 1.5 times of:
  {H1C,H1D} of O1
2. Restrained distances
 O2-H2D
 0.82 with sigma of 0.02
 O2-H2C
 0.82 with sigma of 0.02
3. Others
 Fixed Sof: H6A(0.5) H6B(0.5)
4.a Free rotating group:
 O1(H1C,H1D)
4.b Rotating group with stretchable bonds:
 O2(H2C,H2D)
4.c Ternary CH refined with riding coordinates:
 N5(H5), N4(H4), N1(H1)
4.d Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), C9(H9A,H9B), C1(H1A,H1B), C10(H10A,H10B), C12(H12A,H12B), C7(H7A,
 H7B), C2(H2A,H2B), C8(H8A,H8B), C11(H11A,H11B), C6(H6C,H6D)
4.e Aromatic/amide H refined with riding coordinates:
 C4(H4A)
;
_shelx_res_checksum              70912
_olex2_submission_special_instructions 'No special instructions were received'