Enhancement of magnetic anisotropy in a Mn-Bi heterobimetallic complex.
Pearson, Tyler J.; Fataftah, Majed S.; Freedman, Danna E.; Chemical communications (Cambridge, England) 52 (2016) 11394–11397; doi:10.1039/c6cc06369a

data_7125044
_publ_section_title
;
 Enhancement of magnetic anisotropy in a Mn-Bi heterobimetallic complex.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11394
_journal_page_last               11397
_journal_paper_doi               10.1039/c6cc06369a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C30 H30 Bi F3 Mn N3 O9 S, C1 F3 O3 S1'
_chemical_formula_sum            'C31 H30 Bi F6 Mn N3 O12 S2'
_chemical_formula_weight         1078.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-31 deposited with the CCDC.
2016-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                96.095(3)
_cell_angle_beta                 105.256(3)
_cell_angle_gamma                104.605(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6023(5)
_cell_length_b                   12.8674(7)
_cell_length_c                   15.9332(9)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.37
_cell_measurement_theta_min      2.29
_cell_volume                     1806.25(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73675
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.233
_diffrn_reflns_theta_min         1.348
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.427
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0663 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.9109.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_description       block
_exptl_crystal_F_000             1054
_exptl_crystal_recrystallization_method
'vapor diffusion of diethyl ether into a saturated solution in acetonitrile'
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.034
_refine_diff_density_max         3.842
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10716
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0376P)^2^+1.5933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9198
_reflns_number_total             10716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06369a2.cif
_cod_data_source_block           initsol
_cod_original_cell_volume        1806.25(17)
_cod_database_code               7125044
_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. Restrained distances
 S2A-C31A \\sim S2B-C31B
 with sigma of 0.02
 F4B-F6B \\sim F6B-F5B
 with sigma of 0.02
 F6A-F5A \\sim F5A-F4A
 with sigma of 0.02
 F4B-C31B \\sim F6B-C31B \\sim F5B-C31B \\sim F6A-C31A \\sim F5A-C31A \\sim
F4A-C31A
 with sigma of 0.02
 S2B-O12B \\sim S2B-O11B \\sim S2B-O10B \\sim S2A-O10A \\sim S2A-O12A \\sim
S2A-O11A
 with sigma of 0.02
 O11B-O12B \\sim O12B-O10B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10A \\sim O11B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
O11A \\sim O12B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
F6A \\sim F6B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F5A \\sim F5B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C31A \\sim C31B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O11B) = Uanis(O10A)
Uanis(F6B) = Uanis(F6A)
Uanis(O11A) = Uanis(O12B)
Uanis(F5B) = Uanis(F5A)
Uanis(F4B) = Uanis(F4A)
4. Rigid body (RIGU) restrains
 O10A, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11A, O12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6A, F6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(C31A)=1-
 FVAR(1)
 Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=Sof(C31B)=
 FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C12(H12A,H12B), C21(H21A,H21B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C9(H9), C10(H10), C13(H13), C17(H17), C18(H18), C19(H19),
 C22(H22), C26(H26), C27(H27), C28(H28)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              61438
_shelx_hkl_checksum              42164
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id LMnBi(OTf)2
_olex2_submission_special_instructions 'No special instructions were received'