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_4515169
_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         'C18 H20 Mg N3 Ni O8, N O3'
_chemical_formula_sum            'C18 H20 Mg N4 Ni O11'
_chemical_formula_weight         551.40
_chemical_name_common            'Nickel(II) Magnesium(II) dimethoxysalen'
_chemical_name_systematic        'Nickel(II) Magnesium(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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                83.169(8)
_cell_angle_beta                 84.590(8)
_cell_angle_gamma                85.070(8)
_cell_formula_units_Z            2
_cell_length_a                   8.2292(8)
_cell_length_b                   11.4209(11)
_cell_length_c                   11.5013(11)
_cell_measurement_reflns_used    11087
_cell_measurement_temperature    200
_cell_measurement_theta_max      1.68
_cell_measurement_theta_min      25.50
_cell_volume                     1065.44(18)
_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 1.000
_diffrn_measured_fraction_theta_max 0.983
_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_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.358
_diffrn_reflns_theta_min         1.790
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.2423
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_recrystallization_method 'ether slow diffusion'
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0962P)^2^+0.3801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2964
_reflns_number_total             4280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00365_si_005.cif
_cod_data_source_block           nimgboni_pl_tw
_cod_database_code               4515169
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.743(3)
 0.257(3)
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, All O(H,H) groups
3.a Riding coordinates:
 O8(H8A,H8B)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C13(H13), C14(H14), C15(H15)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              84607
_shelx_hkl_checksum              16892
_olex2_submission_original_sample_id LNiMg
_olex2_submission_special_instructions 'No special instructions were received'