Structural Studies of Manganese(III) Complex with Spin-Crossover and Thermochromic Properties
Villaman, David; McMonagle, Charles J.; Probert, Michael; Peña, Octavio; Moreno, Yanko; Fuentealba, Mauricio; CrystEngComm  (2020) –; doi:10.1039/C9CE01962F

data_7240232
_publ_section_title
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 Structural Studies of Manganese(III) Complex with Spin-Crossover and
 Thermochromic Properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01962F
_journal_year                    2020
_chemical_formula_moiety         'C24 H32 Mn N4 O4, Cl'
_chemical_formula_sum            'C24 H32 Cl Mn N4 O4'
_chemical_formula_weight         530.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.780(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5505(15)
_cell_length_b                   8.4609(17)
_cell_length_c                   19.059(4)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.54
_cell_volume                     1213.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35540
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         28.016
_diffrn_reflns_theta_min         2.544
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1324 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.8991.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.706
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         5025
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0389P)^2^+2.6216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3604
_reflns_number_total             5025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01962f2.cif
_cod_data_source_block           test
_cod_database_code               7240232
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.924
_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. Restrained distances
 N2-C12
 1.469 with sigma of 0.005
 C12A-C12
 1.524 with sigma of 0.005
 N2-C12A_$1
 1.469 with sigma of 0.005
 O1A-C1 \\sim O1A-C1A
 with sigma of 0.001
 O1A-C2 \\sim O1-C2
 with sigma of 0.001
 O1-C2 \\sim O1A-C2
 with sigma of 0.001
 O1A-C1A \\sim O1-C1
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C12A) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.02
Uanis(C12A) = Uanis(C12)
Uanis(C1A) = Uanis(C1)
Uanis(O1) = Uanis(O1A)
4. Others
 Sof(O1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=1-FVAR(1)
 Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
 Fixed Sof: C12(0.5) H12A(0.5) H12B(0.5) C12A(0.5) H12C(0.5) H12D(0.5)
5.a Ternary CH refined with riding coordinates:
 N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C12A(H12C,H12D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C8(H8)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              39719
_olex2_submission_special_instructions 'No special instructions were received'