Pre- and post-synthetic modulation of the ordering temperatures in a family of anilato-based magnets.
Martínez-Hernández, Cristian; Gómez-Claramunt, Patricia; Benmansour, Samia; Gómez-García, Carlos J; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13212–13223; doi:10.1039/c9dt02275a

data_7701776
_publ_section_title
;
 Pre- and post-synthetic modulation of the ordering temperatures in a
 family of anilato-based magnets.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13212
_journal_page_last               13223
_journal_paper_doi               10.1039/c9dt02275a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'Br6 C18 Cr Mn O12, C16 H36 N, C6 H5 Br'
_chemical_formula_sum            'C40 H41 Br7 Cr Mn N O12'
_chemical_formula_weight         1394.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-07-10
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2019-07-16 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.187(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9557(5)
_cell_length_b                   23.6054(10)
_cell_length_c                   12.2129(6)
_cell_measurement_reflns_used    5983
_cell_measurement_temperature    119.6(8)
_cell_measurement_theta_max      24.9817
_cell_measurement_theta_min      3.3398
_cell_volume                     2769.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -84.00    6.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9661  -57.0000    0.0000 90

  2 omega  -20.00   27.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9661  -99.0000  -90.0000 47

  3 omega  -10.00   84.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255   70.0000 -110.0000 94

  4 omega  -53.00   37.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -57.0000    0.0000 90

  5 omega  -49.00   46.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -77.0000  120.0000 95

  6 omega  -40.00  -15.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9661   38.0000  -60.0000 25

  7 omega  -92.00  -34.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9661  178.0000  150.0000 58

  8 omega  -20.00   58.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -99.0000  -90.0000 78

  9 omega  -20.00   58.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -99.0000   30.0000 78

 10 omega  -53.00   37.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -57.0000  150.0000 90

 11 omega   -6.00   85.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       15.8255   57.0000  150.0000 91
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41361
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.035
_diffrn_reflns_theta_max         25.035
_diffrn_reflns_theta_min         3.347
_exptl_absorpt_coefficient_mu    5.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       plate
_exptl_crystal_F_000             1356
_exptl_crystal_recrystallization_method
'The material was recrystallised from  by solvent layering'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9776
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+11.7191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2222
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7412
_reflns_number_total             9776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02275a2.cif
_cod_data_source_block           crys196d
_cod_database_code               7701776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.67(3)
 0.33(3)
2. 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
3. Restrained distances
 C1C-C3C \\sim C3D-C1D \\sim C1B-C3B \\sim C1A-C3A
 with sigma of 0.0001
 C7-C2D \\sim C4B-C2B \\sim C4C-C2C \\sim C4A-C2A
 with sigma of 0.0001
 C3B-C2B \\sim C4B-C3B
 with sigma of 0.0001
4. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O22, Cr1, O2, O3, O12, O13, O23, C2, C3, C12, C13, C22, C23, C1, C4, C11, C14,
  C21, C24, C6, Br1, C5, Br4, Br11, C16, Br14, C15, Br21, C26, Br24, C25, O6,
 O5, O16, O15, O26, O25, Mn1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Br1H, C1H, C2H, C6H, C3H, C5H, C4H
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, N1T, C1B, C1C, C1D, C2A, C2B, C2C, C2D, C3A, C3B, C3C, C3D, C4A, C4B,
 C4C, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Uiso: C7(0.12)
 Fixed X: C7(0.96358)
 Fixed Y: C7(0.674049)
 Fixed Z: C7(0.324381)
7.a Riding coordinates:
 C7(H7A,H7B,H7C)
7.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C1B(H1BA,H1BB), C2B(H2BA,
 H2BB), C3B(H3BA,H3BB), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C3C(H3CA,H3CB),
 C1D(H1DA,H1DB), C2D(H2DA,H2DB), C3D(H3DA,H3DB)
7.c Aromatic/amide H refined with riding coordinates:
 C2H(H2H), C3H(H3H), C4H(H4H), C5H(H5H), C6H(H6H)
7.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C1H(C2H,C3H,C4H,C5H,C6H)
7.e Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC), C4C(H4CA,H4CB,H4CC)
;
_shelx_res_checksum              54158
_shelx_fab_checksum              85034
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'