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_7713976
_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         'C33 H43 Br2 Co N3, H2 O'
_chemical_formula_sum            'C33 H45 Br2 Co N3 O'
_chemical_formula_weight         718.47
_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   mixed
_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                83.553(4)
_cell_angle_beta                 88.087(4)
_cell_angle_gamma                65.722(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7050(4)
_cell_length_b                   10.0376(6)
_cell_length_c                   20.8391(8)
_cell_measurement_reflns_used    6859
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.8390
_cell_measurement_theta_min      2.7390
_cell_volume                     1649.17(15)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.868
_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    -63.00  -8.00   0.50   35.00    --    7.20 -82.00  30.00  110
  2  \w      0.00  46.00   0.50   35.00    --    7.20 -82.00  30.00   92
  3  \w     46.00  88.00   0.50   35.00    --    7.20  57.00 120.00   84
  4  \w     50.00  97.00   0.50   35.00    --    7.20  77.00 -90.00   94
  5  \w     57.00  84.00   0.50   35.00    --    7.20  77.00  60.00   54
  6  \w     66.00  97.00   0.50   35.00    --    7.20  77.00   0.00   62
  7  \w    -57.00  25.00   0.50   35.00    --   -7.60 -82.00-150.00  164
  8  \w    -47.00  22.00   0.50   35.00    --   -7.60 -82.00 -30.00  138
  9  \w     -3.00  24.00   0.50   35.00    --   -7.60 -82.00 -90.00   54
 10  \w    -61.00 -25.00   0.50   35.00    --   -7.60 -82.00 -90.00   72
 11  \w    -63.00   7.00   0.50   35.00    --   -7.60 -82.00 120.00  140
;
_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      -0.0583277000
_diffrn_orient_matrix_UB_12      -0.0250628000
_diffrn_orient_matrix_UB_13      0.0156578000
_diffrn_orient_matrix_UB_21      0.0541823000
_diffrn_orient_matrix_UB_22      -0.0286956000
_diffrn_orient_matrix_UB_23      0.0275001000
_diffrn_orient_matrix_UB_31      -0.0406659000
_diffrn_orient_matrix_UB_32      0.0680361000
_diffrn_orient_matrix_UB_33      0.0131194000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23924
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.047
_diffrn_reflns_theta_min         2.624
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39892
_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    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0650
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4757
_reflns_number_total             7632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01769a2.cif
_cod_data_source_block           aj_1957
_cod_database_code               7713976
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCoBr
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.602
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.036) H3(0.047) H4(0.042) H9A(0.058) H9B(0.058) H9C(0.058)
 H26(0.046) H14(0.049) H12(0.047) H31(0.046) H13(0.051) H24(0.05) H19(0.049)
 H25(0.057) H16(0.049) H28(0.057) H20A(0.086) H20B(0.086) H20C(0.086)
 H7A(0.064) H7B(0.064) H7C(0.064) H21A(0.092) H21B(0.092) H21C(0.092)
 H17A(0.087) H17B(0.087) H17C(0.087) H29A(0.102) H29B(0.102) H29C(0.102)
 H33A(0.106) H33B(0.106) H33C(0.106) H18A(0.093) H18B(0.093) H18C(0.093)
 H32A(0.106) H32B(0.106) H32C(0.106) H30A(0.129) H30B(0.129) H30C(0.129)
 H1A(0.306) H1B(0.306)
 Fixed X: H2(0.565765) H3(0.701421) H4(0.817252) H9A(0.365911) H9B(0.553967)
 H9C(0.429005) H26(0.741067) H14(0.11081) H12(0.590813) H31(0.540675)
 H13(0.309428) H24(1.102418) H19(0.187408) H25(0.977245) H16(0.76888)
 H28(0.96085) H20A(0.146141) H20B(-0.014535) H20C(-0.007433) H7A(0.952257)
 H7B(0.994965) H7C(0.843381) H21A(-0.063355) H21B(-0.08474) H21C(0.043089)
 H17A(0.84562) H17B(0.965284) H17C(0.799352) H29A(0.993109) H29B(1.126781)
 H29C(1.17794) H33A(0.435289) H33B(0.316389) H33C(0.41101) H18A(0.76369)
 H18B(0.941437) H18C(0.813913) H32A(0.681366) H32B(0.487334) H32C(0.609894)
 H30A(1.270181) H30B(1.247934) H30C(1.159357) H1A(0.382299) H1B(0.31056)
 Fixed Y: H2(0.793507) H3(0.831433) H4(0.645685) H9A(0.731623) H9B(0.659658)
 H9C(0.589864) H26(-0.015361) H14(0.370927) H12(0.126476) H31(0.336749)
 H13(0.202764) H24(-0.189633) H19(0.548852) H25(-0.208663) H16(0.248441)
 H28(0.119169) H20A(0.333916) H20B(0.478432) H20C(0.383343) H7A(0.281261)
 H7B(0.399616) H7C(0.448924) H21A(0.59155) H21B(0.695875) H21C(0.685617)
 H17A(0.004274) H17B(0.017183) H17C(0.00095) H29A(-0.122756) H29B(-0.079294)
 H29C(-0.18191) H33A(0.135166) H33B(0.294224) H33C(0.172724) H18A(0.381413)
 H18B(0.251703) H18C(0.238049) H32A(0.33317) H32B(0.38794) H32C(0.226768) H30A(-
 0.015864) H30B(0.070453) H30C(0.153838) H1A(0.028362) H1B(0.097281)
 Fixed Z: H2(0.782435) H3(0.68981) H4(0.622596) H9A(0.865111) H9B(0.889348)
 H9C(0.914655) H26(0.507245) H14(0.95896) H12(1.007313) H31(0.567027)
 H13(1.02991) H24(0.642141) H19(0.811373) H25(0.55171) H16(0.868426)
 H28(0.732045) H20A(0.795016) H20B(0.775954) H20C(0.841741) H7A(0.56481)
 H7B(0.593919) H7C(0.545172) H21A(0.906966) H21B(0.842868) H21C(0.896431)
 H17A(0.963712) H17B(0.907755) H17C(0.892022) H29A(0.770412) H29B(0.80025)
 H29C(0.744659) H33A(0.519975) H33B(0.535391) H33C(0.59165) H18A(0.954336)
 H18B(0.950038) H18C(1.002519) H32A(0.469893) H32B(0.457297) H32C(0.446172)
 H30A(0.669702) H30B(0.730004) H30C(0.664201) H1A(0.909199) H1B(0.849368)
;
_shelx_res_checksum              60342
_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 2.211
_oxdiff_exptl_absorpt_empirical_full_min 0.408