Investigation of the magnetic anisotropy in a series of trigonal bipyramidal Mn(ii) complexes.
Hay, Moya A.; Sarkar, Arup; Marriott, Katie E. R.; Wilson, Claire; Rajaraman, Gopalan; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15480–15486; doi:10.1039/c9dt02187f

data_7701639
_publ_section_title
;
 Investigation of the magnetic anisotropy in a series of trigonal
 bipyramidal Mn(ii) complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15480
_journal_page_last               15486
_journal_paper_doi               10.1039/c9dt02187f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C7 H17 Cl3 Mn N2 O'
_chemical_formula_sum            'C7 H17 Cl3 Mn N2 O'
_chemical_formula_weight         306.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.572(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8885(19)
_cell_length_b                   9.447(3)
_cell_length_c                   8.269(2)
_cell_measurement_reflns_used    1590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.55
_cell_measurement_theta_min      2.60
_cell_volume                     612.2(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1121
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.683
_diffrn_reflns_theta_min         2.479
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1178 before and 0.0980 after correction.
The Ratio of minimum to maximum transmission is 0.8193.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       needle
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0380P)^2^+0.8815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1004
_reflns_number_total             1236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02187f2.cif
_cod_data_source_block           complex3
_cod_database_code               7701639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1a,H1b} of C1, {H2a,H2b} of C2, {H4a,H4b} of C4, {H3a,H3b} of C3
 At 1.5 times of:
  {H5a,H5b} of C5
2. Restrained distances
 C5-H5b = C5-H5a
 0.98 with sigma of 0.02
 C5-H5a = C5-H5b
 0.96 with sigma of 0.02
3. Others
 Fixed Sof: H1a(0.5) H1b(0.5) H2a(0.5) H2b(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b)
;
_shelx_res_checksum              31137
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'