Modulation of the spin crossover behaviour in four manganese(III) complexes through cation-anion interactions.
Malik, Suvamoy; Brandão, Paula; Benmansour, Samia; Gómez-García, Carlos J; Saha, Amrita; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6645–6652; doi:10.1039/d5dt00238a

data_7718334
_publ_section_title
;
 Modulation of the spin crossover behaviour in four manganese(III)
 complexes through cation-anion interactions.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6645
_journal_page_last               6652
_journal_paper_doi               10.1039/d5dt00238a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C29.5 H39.5 Mn N4 O4, F6 P, 0.5(C)'
_chemical_formula_sum            'C30 H40 F6 Mn N4 O4 P'
_chemical_formula_weight         720.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-09-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-17 deposited with the CCDC.	2025-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.616(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.188(4)
_cell_length_b                   13.798(3)
_cell_length_c                   11.8038(19)
_cell_measurement_reflns_used    464
_cell_measurement_temperature    295.00
_cell_measurement_theta_max      27.104
_cell_measurement_theta_min      1.872
_cell_volume                     3323.5(11)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      295.00
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            64705
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.193
_diffrn_reflns_theta_min         2.329
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0.998
_exptl_transmission_factor_min   0.992
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.024(6)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.393
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0551
_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^)+(0.1110P)^2^+2.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3201
_reflns_number_total             3610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00238a2.cif
_cod_data_source_block           complex1_rt
_cod_depositor_comments
'Adding full bibliography for 7718333--7718340.cif.'
_cod_original_cell_volume        3323.4(10)
_cod_database_code               7718334
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C10) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P1) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F12)
\\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 C19, C16, C17, C18, C9, C8, C10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9(0.5) C10(0.5) H10A(0.5)
 H10B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C16(0.25) C18(0.25) H18(0.25) C19(0.5)
 H19A(0.5) H19B(0.5)
5.a Ternary CH refined with riding coordinates:
 N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C8(H8A,H8B),
 C19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C9(H9), C18(H18)
5.d X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B)
5.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              87060
_shelx_hkl_checksum              59757
_olex2_submission_special_instructions 'No special instructions were received'