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_4515166
_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         '2(C36 H34 Ba N6 Ni2 O14)'
_chemical_formula_sum            'C72 H68 Ba2 N12 Ni4 O28'
_chemical_formula_weight         2058.90
_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             2019-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                100.388(17)
_cell_angle_beta                 92.814(18)
_cell_angle_gamma                90.137(16)
_cell_formula_units_Z            2
_cell_length_a                   11.632(2)
_cell_length_b                   16.114(3)
_cell_length_c                   23.382(6)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      1.69
_cell_volume                     4305.4(16)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.3528
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_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       -25
_diffrn_reflns_number            15400
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_min         1.285
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    1.839
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_correction_T_min  0.6850
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by slow evaporation'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.017
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.00048(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         15400
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.2806
_refine_ls_R_factor_gt           0.0932
_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^)+(0.0738P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4260
_reflns_number_total             15400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00365_si_008.cif
_cod_data_source_block           niba_tw_sq
_cod_original_cell_volume        4305.2(16)
_cod_database_code               4515166
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.964
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.729(4)
 0.271(4)
2. 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
3. Restrained distances
 N12-O32
 1.25 with sigma of 0.02
 N12-O34
 1.25 with sigma of 0.02
 N12-O33
 1.25 with sigma of 0.02
 O22-N10
 1.25 with sigma of 0.02
4. Restrained planarity
 O32, N12, O33, O34
 with sigma of 0.1
5. Rigid bond restraints
 C48, C53, C52, C51, C50, C49
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C53, C48, C49, C50, C52, C51
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N11, O26, O27, O28
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N9, O17, O18, O19
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C7, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C24, C23, C22, C21, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59, C58, C57, C56, C61, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C62, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C66, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C36) = Uanis(C19) = Uanis(C18) = Uanis(C72) = Uanis(C54) =
Uanis(C55) = Uanis(C37)
Uanis(C46) = Uanis(C45) = Uanis(C10) = Uanis(C9) = Uanis(C27) = Uanis(C28) =
Uanis(C63) = Uanis(C64)
Uanis(O31) = Uanis(O33) = Uanis(O30) = Uanis(O34) = Uanis(O29) = Uanis(O32)
Uanis(O23) = Uanis(O20) = Uanis(O24) = Uanis(O21) = Uanis(O25) = Uanis(O22)
Uanis(O17) = Uanis(O18) = Uanis(O19)
7. Others
 Sof(O29)=Sof(O31)=Sof(O30)=1-FVAR(1)
 Sof(O32)=Sof(O34)=Sof(O33)=FVAR(1)
 Sof(O23)=Sof(O24)=Sof(O25)=1-FVAR(2)
 Sof(O20)=Sof(O21)=Sof(O22)=FVAR(2)
8.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C64(H64A,H64B), C9(H9A,H9B), C63(H63A,H63B)
8.b Aromatic/amide H refined with riding coordinates:
 C57(H57), C13(H13), C44(H44), C11(H11), C39(H39), C23(H23), C27(H27),
 C29(H29), C33(H33), C26(H26), C3(H3), C41(H41), C31(H31), C58(H58), C51(H51),
 C8(H8), C59(H59), C40(H40), C4(H4), C32(H32), C14(H14), C47(H47), C67(H67),
 C49(H49), C65(H65), C62(H62), C15(H15), C5(H5), C50(H50), C69(H69), C22(H22),
 C68(H68), C21(H21), C45(H45), C46(H46), C28(H28)
8.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C55(H55A,H55B,H55C), C72(H72A,H72B,H72C), C54(H54A,H54B,
 H54C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              88506
_shelx_hkl_checksum              77308
_shelx_fab_checksum              86017
_platon_squeeze_void_probe_radius 1.20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop in oil'
_olex2_submission_original_sample_id LNiBa
_olex2_submission_special_instructions 'No special instructions were received'