Structure and magnetic characterization of some bicompartmental [N6O2] divalent metal(ii) complexes using bis(phenolato) ligands bearing two pendant bis(pyridyl) amine arms
Mautner, Franz A.; Fischer, Roland C.; Torvisco, Ana; Nakashima, Kai; Handa, Makoto; Mikuriya, Masahiro; Salem, Nahed M. H.; Overby, Gabriel J.; Maier, Madison R.; Louka, Febee R.; Massoud, Salah S.; New Journal of Chemistry 47 (2023) 15638–15649; doi:10.1039/D3NJ02380J

data_7062658
_publ_section_title
;
 Structure and magnetic characterization of some bicompartmental [N6O2]
 divalent metal(ii) complexes using bis(phenolato) ligands bearing two
 pendant bis(pyridyl) amine arms
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15638
_journal_page_last               15649
_journal_paper_doi               10.1039/D3NJ02380J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C43 H43 Cd2 Cl2 N6 O7, F6 P, H2 O'
_chemical_formula_sum            'C43 H45 Cd2 Cl2 F6 N6 O8 P'
_chemical_formula_weight         1214.52
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-05-20 deposited with the CCDC.	2023-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.122(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1145(9)
_cell_length_b                   14.5430(7)
_cell_length_c                   20.9676(10)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.22
_cell_volume                     5102.4(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1267
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            141635
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         1.717
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.97
_diffrn_source_power             0.0485
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1393 before and 0.0978 after correction.
The Ratio of minimum to maximum transmission is 0.7041.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         11704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0064P)^2^+7.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8526
_reflns_number_total             11704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02380j2.cif
_cod_data_source_block           rf2085a_0m
_cod_depositor_comments
'Adding full bibliography for 7062656--7062659.cif.'
_cod_database_code               7062658
_shelx_shelxl_version_number     2014/7
_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 O(H,H) groups
2.a Free rotating group:
 O7(H7C,H7D)
2.b Rotating group:
 O5(H5A,H5B)
2.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C14(H14A,H14B), C20(H20A,H20B), C27(H27A,H27B),
 C28(H28A,H28B), C34(H34A,H34B)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C11(H11), C13(H13), C12(H12), C16(H16), C18(H18),
 C17(H17), C19(H19), C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33),
  C36(H36), C37(H37), C38(H38), C39(H39)
2.e Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              10807
_olex2_submission_special_instructions 'No special instructions were received'