Compartmentalization of Alkaline-Earth Metals in Salen-Type Cu- and Ni-Complexes in Solution and in the Solid State.
Finelli, Alba; Hérault, Nelly; Crochet, Aurélien; Fromm, Katharina M.; ACS omega 4 (2019) 10231–10242; doi:10.1021/acsomega.9b00365

data_4515163
_publ_section_title
;
 Compartmentalization of Alkaline-Earth Metals in Salen-Type Cu- and
 Ni-Complexes in Solution and in the Solid State.
;
_journal_issue                   6
_journal_name_full               'ACS omega'
_journal_page_first              10231
_journal_page_last               10242
_journal_paper_doi               10.1021/acsomega.9b00365
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C36 H36 Ba Cu2 N6 O14'
_chemical_formula_sum            'C36 H36 Ba Cu2 N6 O14'
_chemical_formula_weight         1041.12
_chemical_name_systematic        'Copper(II) Barium(II) dimethoxysalen'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                79.040(4)
_cell_angle_beta                 87.041(4)
_cell_angle_gamma                89.654(4)
_cell_formula_units_Z            4
_cell_length_a                   11.6329(5)
_cell_length_b                   16.1304(7)
_cell_length_c                   23.2105(11)
_cell_measurement_reflns_used    28456
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      1.29
_cell_volume                     4270.1(3)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1289
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55027
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         1.286
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_recrystallization_method 'Slow evaporation ACN/EtOH'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         15205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9584
_reflns_number_total             15205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00365_si_004.cif
_cod_data_source_block           af104a-5cuba_sq
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C36 H36 Ba Cu2 N6 O14)'
_cod_original_formula_sum        'C72 H72 Ba2 Cu4 N12 O28'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2082.25
_cod_database_code               4515163
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C27(H27A,H27B), C28(H28A,H28B), C45(H45A,H45B),
 C46(H46A,H46B), C63(H63A,H63B), C64(H64A,H64B)
2.b Aromatic/amide H refined with riding coordinates:
 C01Q(H01Q), C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C13(H13), C14(H14),
 C15(H15), C21(H21), C22(H22), C23(H23), C26(H26), C31(H31), C32(H32), C33(H33),
  C39(H39), C40(H40), C41(H41), C44(H44), C47(H47), C49(H49), C50(H50),
 C51(H51), C57(H57), C58(H58), C59(H59), C62(H62), C65(H65), C67(H67), C68(H68),
  C69(H69)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C72(H72A,
 H72B,H72C)
;
_shelx_res_checksum              61760
_shelx_hkl_checksum              55119
_shelx_fab_checksum              94887
_olex2_submission_original_sample_id LCuBa
_olex2_submission_special_instructions 'No special instructions were received'