Multinuclear Ni(ii), Cu(ii) and Zn(ii) complexes of chiral macrocyclic nonaazamine.
Löffler, Marta; Gregoliński, Janusz; Korabik, Maria; Lis, Tadeusz; Lisowski, Jerzy; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15586–15594; doi:10.1039/c6dt02504h

data_7040548
_publ_section_title
;
 Multinuclear Ni(ii), Cu(ii) and Zn(ii) complexes of chiral macrocyclic
 nonaazamine.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15586
_journal_page_last               15594
_journal_paper_doi               10.1039/c6dt02504h
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C39 H61 Cl5 N9 Ni3 O2, 0.4(C2 H3 N), Cl, 4.2(H2 O)'
_chemical_formula_sum            'C39.8 H70.6 Cl6 N9.4 Ni3 O6.2'
_chemical_formula_weight         1168.88
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.592(5)
_cell_length_b                   15.270(7)
_cell_length_c                   24.284(12)
_cell_measurement_reflns_used    4400
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4997
_cell_measurement_theta_min      2.7909
_cell_volume                     5040(4)
_computing_cell_refinement
'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_data_collection
'CrysAlis CCD; Oxford-Diffraction Poland, 2003'
_computing_data_reduction
'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.2711
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24969
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.797
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
               model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             2443
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 1518 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.024(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         11274
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1728
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0050P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                5183
_reflns_number_total             11274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02504h2.cif
_cod_data_source_block           NID6LA
_cod_depositor_comments
;Adding full bibliography for 7040547--7040549.cif.

 Adding full bibliography for 7040547--7040549.cif.
;
_cod_original_formula_sum        'C39.80 H70.60 Cl6 N9.40 Ni3 O6.20'
_cod_database_code               7040548
_shelx_estimated_absorpt_t_min   0.665
_shelx_estimated_absorpt_t_max   0.916
_shelxl_version_number           2013-2
_shelx_res_checksum              29436