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_4515162
_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 H18 Ca Cu N4 O10'
_chemical_formula_sum            'C18 H18 Ca Cu N4 O10'
_chemical_formula_weight         553.98
_chemical_name_systematic        'Copper(II) Calcium(II) dimethoxysalen'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.441(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7160(6)
_cell_length_b                   12.8272(7)
_cell_length_c                   13.7268(7)
_cell_measurement_reflns_used    12330
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.17
_cell_volume                     2062.26(19)
_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 1.000
_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  0.1106
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_process_details
'Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1132
_exptl_crystal_recrystallization_method 'Slow evaporation ACN/EtOH'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0630P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2380
_reflns_number_total             3633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00365_si_002.cif
_cod_data_source_block           af121-5cuca
_cod_database_code               4515162
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.852
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C13(H13), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              18836
_shelx_hkl_checksum              74669
_olex2_exptl_crystal_mounting_method '2-circle goniometer'
_olex2_submission_original_sample_id LCuCa
_olex2_submission_special_instructions 'No special instructions were received'