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_4515168
_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 Cu N4 O11 Sr'
_chemical_formula_sum            'C18 H20 Cu N4 O11 Sr'
_chemical_formula_weight         619.54
_chemical_name_systematic        'Copper(II) Strontium(II) dimethoxysalen'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7055(5)
_cell_length_b                   8.6682(5)
_cell_length_c                   11.1732(14)
_cell_measurement_reflns_used    11535
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      1.79
_cell_volume                     2199.1(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0780
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26728
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  0.8485
_exptl_absorpt_correction_T_min  0.5795
_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    1.871
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1244
_exptl_crystal_recrystallization_method 'Slow Diffusion ACN/EtOH-diethyl ether'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 1066 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(5)
_refine_ls_extinction_coef       0.0028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3809
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0450P)^2^+0.8623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                2817
_reflns_number_total             3809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00365_si_003.cif
_cod_data_source_block           af47lg5cusr
_cod_database_code               4515168
_shelx_shelxl_version_number     2018/3
_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, All Sr(H,H) groups
2. Restrained distances
 H11B-O11
 0.91 with sigma of 0.02
 O11-H11A
 0.91 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) = Uanis(O6) = Uanis(O8) = Uanis(O9)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C8(H8), C11(H11), C15(H15), C14(H14), C13(H13)
4.c Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C3,C2), C17(C16,C15,C14,C13,C12)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              54222
_shelx_hkl_checksum              28635
_olex2_submission_original_sample_id LCuSr
_olex2_submission_special_instructions 'No special instructions were received'