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_7704620
_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
'C28 H56 Cu1.62 N12 O2 Pd2.38, 2(Cl O4), 0.67(Br), 1.33(Cl), 1.87(H2 O), O'
_chemical_formula_sum
'C28 H59.75 Br0.67 Cl3.33 Cu1.61 N12 O12.87 Pd2.39'
_chemical_formula_weight         1298.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2020-06-01 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.852(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8708(7)
_cell_length_b                   19.3357(11)
_cell_length_c                   19.8511(7)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      26.9130
_cell_measurement_theta_min      3.8300
_cell_volume                     4775.2(4)
_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)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.868
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12151
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.932
_diffrn_reflns_theta_min         3.175
_exptl_absorpt_coefficient_mu    2.404
_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.476
_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_density_diffrn    1.807
_exptl_crystal_description       block
_exptl_crystal_F_000             2606
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.352
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6176
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1194P)^2^+31.7132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4214
_reflns_number_total             6176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01056a2.cif
_cod_data_source_block           4_pdcu
_cod_depositor_comments
'Adding full bibliography for 7704616--7704620.cif.'
_cod_database_code               7704620
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.585
_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 N(H,H) groups, All
  O(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O12-H3C
 2 with sigma of 0.02
 O3-H3D = O3-H3C
 0.85 with sigma of 0.02
 O1-H1
 0.97 with sigma of 0.01
 N3B-Cu1
 2.1 with sigma of 0.01
 N3B-C6B
 1.5 with sigma of 0.02
 C6B-C5B
 1.53 with sigma of 0.02
 C6-C5
 1.53 with sigma of 0.02
 C5-C4
 1.54 with sigma of 0.02
 C5B-C4B
 1.54 with sigma of 0.02
 C4-N2
 1.49 with sigma of 0.02
 C4B-N2
 1.49 with sigma of 0.02
 C7B-N3B
 1.49 with sigma of 0.02
 C8B-C7B
 1.51 with sigma of 0.01
 C7B-C7B_$1
 2.3 with sigma of 0.01
 Pd2-N3
 2.08 with sigma of 0.01
 N3-C7
 1.49 with sigma of 0.02
 N3-C6
 1.5 with sigma of 0.02
 C8-C7
 1.51 with sigma of 0.01
 O2-H2
 0.82 with sigma of 0.01
 H3D-H3C
 1.33 with sigma of 0.04
3. Rigid bond restraints
 C7B, C8B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C7, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C6B, C5B, C4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7B, N3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3B, C6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(Cu1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(Cu1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C7) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.006
Uanis(Pd2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8B) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(N3B) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Cu2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Sof(H2B)=Sof(N3)=Sof(H3)=Sof(C6)=Sof(H6C)=Sof(H6D)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=Sof(H7B)=1-FVAR(1)
 Sof(Pd2)=Sof(C8)=Sof(H8A)=Sof(H8B)=0.5*(1-FVAR(2))
 Sof(Cu1)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=0.5*FVAR(2)
 Sof(H2A)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(N3B)=Sof(H3BA)=Sof(C6B)=Sof(H6BA)=
 Sof(H6BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=FVAR(1)
 Sof(O2)=0.5*FVAR(3)
 Sof(H2)=FVAR(2)
 Fixed Sof: Br1(0.33333) H6A(0.5) H6B(0.5) Cl3(0.16667) O3(0.75) H3C(0.75)
 H3D(0.75) O4(0.5)
6.a Rotating group with stretchable bonds:
 O1(H1), O2(H2)
6.b Ternary CH refined with riding coordinates:
 N5(H5), N2(H2B), N2(H2A), N3(H3), N3B(H3BA)
6.c Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), C13(H13A,H13B), C11(H11A,H11B), C14(H14A,H14B), C16(H16A,H16B),
 C15(H15A,H15B), C12(H12A,H12B), C6(H6C,H6D), C5(H5A,H5B), C3(H3A,H3B), C4(H4A,
 H4B), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C7(H7A,H7B), C6B(H6BA,H6BB), C5B(H5BA,
 H5BB), C4B(H4BA,H4BB), C8(H8A,H8B)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C1(H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'