Field Induced Single Ion Magnet Behavior in CoII Complexes in Distorted Square Pyramidal Geometry
Dey, Atanu; Ali, Junaid; MOORTHY, SHRUTI; Flores-Gonzalez, Jessica; Pointillart, Fabrice; Singh, Saurabh Kumar; Chandrasekhar, Vadapalli; Dalton Transactions  (2023) –; doi:10.1039/D3DT01769A

data_7713974
_publ_section_title
;
 Field Induced Single Ion Magnet Behavior in CoII Complexes in Distorted
 Square Pyramidal Geometry
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01769A
_journal_year                    2023
_chemical_formula_moiety         'C35 H43 Co N5 Se2'
_chemical_formula_sum            'C35 H43 Co N5 Se2'
_chemical_formula_weight         750.59
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-12
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2023-06-07 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.171(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.1187(17)
_cell_length_b                   9.1323(4)
_cell_length_c                   20.1316(9)
_cell_measurement_reflns_used    12524
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.0800
_cell_measurement_theta_min      2.9740
_cell_volume                     7539.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      6.00  31.08   0.38  142.15    --    7.10 -16.00 164.00   66
  2  \w    -75.00 -48.78   0.38  142.15    --    7.10 -16.00 164.00   69
  3  \w     65.00  90.08   0.38  142.15    --    7.10  77.00-180.00   66
  4  \w     58.00  86.50   0.38  142.15    --    7.10  77.00 120.00   75
  5  \w    -23.00  14.24   0.38  142.15    --   -7.50 -57.00   0.00   98
  6  \w    -36.00  79.14   0.38  142.15    --   -7.50  38.00  90.00  303
  7  \w    -34.00  51.12   0.38  142.15    --   -7.50  57.00   0.00  224
  8  \w    -31.00  -6.68   0.38  142.15    --   -7.50  16.00 -25.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0014582000
_diffrn_orient_matrix_UB_12      0.0064514000
_diffrn_orient_matrix_UB_13      0.0356886000
_diffrn_orient_matrix_UB_21      0.0168281000
_diffrn_orient_matrix_UB_22      0.0157605000
_diffrn_orient_matrix_UB_23      0.0045776000
_diffrn_orient_matrix_UB_31      -0.0036394000
_diffrn_orient_matrix_UB_32      0.0757519000
_diffrn_orient_matrix_UB_33      -0.0039791000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35083
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.966
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            deepblue
_exptl_crystal_colour_primary    deepblue
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0776P)^2^+6.5003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5305
_reflns_number_total             8666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01769a2.cif
_cod_data_source_block           aj1904
_cod_database_code               7713974
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Se Co'
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.644
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.08) H4(0.075) H2(0.075) H21A(0.114) H21B(0.114) H21C(0.114)
 H31(0.101) H25(0.1) H19A(0.127) H19B(0.127) H19C(0.127) H28(0.109) H14(0.105)
 H9(0.127) H10(0.109) H16(0.105) H15(0.116) H8(0.121) H22(0.131) H27A(0.182)
 H27B(0.182) H27C(0.182) H30A(0.186) H30B(0.186) H30C(0.186) H32A(0.196)
 H32B(0.196) H32C(0.196) H33A(0.179) H33B(0.179) H33C(0.179) H23A(0.196)
 H23B(0.196) H23C(0.196) H26A(0.174) H26B(0.174) H26C(0.174) H24A(0.226)
 H24B(0.226) H24C(0.226) H29A(0.229) H29B(0.229) H29C(0.229)
 Fixed X: H3(0.413284) H4(0.440145) H2(0.367989) H21A(0.444811) H21B(0.470639)
 H21C(0.454916) H31(0.45381) H25(0.353313) H19A(0.300869) H19B(0.331217)
 H19C(0.311813) H28(0.376891) H14(0.400959) H9(0.237492) H10(0.280656)
 H16(0.465802) H15(0.438965) H8(0.238661) H22(0.306188) H27A(0.313355)
 H27B(0.346575) H27C(0.316182) H30A(0.338178) H30B(0.329141) H30C(0.344684)
 H32A(0.458212) H32B(0.465965) H32C(0.430502) H33A(0.501849) H33B(0.508422)
 H33C(0.506704) H23A(0.270641) H23B(0.264135) H23C(0.240568) H26A(0.359257)
 H26B(0.374285) H26C(0.340224) H24A(0.25112) H24B(0.276483) H24C(0.286879)
 H29A(0.386926) H29B(0.375196) H29C(0.411136)
 Fixed Y: H3(0.210349) H4(0.176467) H2(0.361645) H21A(0.103333) H21B(0.228785)
 H21C(0.196936) H31(0.568045) H25(0.817157) H19A(0.605405) H19B(0.598055)
 H19C(0.455) H28(0.19465) H14(0.246232) H9(0.87803) H10(0.991965) H16(0.560346)
 H15(0.409189) H8(0.631482) H22(0.395888) H27A(1.058005) H27B(1.01804)
 H27C(0.915999) H30A(0.313603) H30B(0.148773) H30C(0.197898) H32A(0.771354)
 H32B(0.810149) H32C(0.765013) H33A(0.457687) H33B(0.613885) H33C(0.591548)
 H23A(0.371725) H23B(0.245819) H23C(0.380775) H26A(0.937891) H26B(1.029664)
 H26C(1.072593) H24A(0.416137) H24B(0.287713) H24C(0.444458) H29A(0.014233)
 H29B(-0.037329) H29C(0.016751)
 Fixed Z: H3(0.661713) H4(0.574364) H2(0.645453) H21A(0.454928) H21B(0.47479)
 H21C(0.397801) H31(0.418199) H25(0.517814) H19A(0.555305) H19B(0.617005)
 H19C(0.590719) H28(0.340186) H14(0.181186) H9(0.354202) H10(0.424371)
 H16(0.248752) H15(0.163305) H8(0.334941) H22(0.398553) H27A(0.533706)
 H27B(0.583536) H27C(0.578425) H30A(0.25397) H30B(0.261249) H30C(0.201095)
 H32A(0.316238) H32B(0.394128) H32C(0.356592) H33A(0.400183) H33B(0.43271)
 H33C(0.354761) H23A(0.470617) H23B(0.416269) H23C(0.408384) H26A(0.416212)
 H26B(0.481631) H26C(0.435891) H24A(0.289536) H24B(0.300947) H24C(0.282248)
 H29A(0.233375) H29B(0.298109) H29C(0.305168)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83358
_shelx_fab_checksum              69684
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.669