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_7713975
_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 Cl2 Co N3, H2 O'
_chemical_formula_sum            'C33 H45 Cl2 Co N3 O'
_chemical_formula_weight         629.55
_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                84.262(2)
_cell_angle_beta                 88.202(2)
_cell_angle_gamma                65.478(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7366(3)
_cell_length_b                   9.9079(3)
_cell_length_c                   20.9732(5)
_cell_measurement_reflns_used    13881
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.5740
_cell_measurement_theta_min      2.7710
_cell_volume                     1643.34(9)
_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      air
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.881
_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    -77.00 -52.00   0.50   17.13    --    7.10 -47.00  91.00   50
  2  \w    -25.00  51.00   0.50   17.13    --    7.10  47.00-119.00  152
  3  \w      2.00  57.00   0.50   17.13    --   -7.50  47.00-119.00  110
  4  \w    -60.00 -35.00   0.50   17.13    --   -7.50 -47.00  91.00   50
  5  \w     50.00  90.00   0.50   17.13    --    7.10  77.00 150.00   80
  6  \w     50.00  95.00   0.50   17.13    --    7.10  77.00 120.00   90
  7  \w     50.00  92.00   0.50   17.13    --    7.10  77.00-180.00   84
  8  \w     50.00  84.00   0.50   17.13    --    7.10  77.00 -90.00   68
  9  \w     52.00  96.00   0.50   17.13    --    7.10  77.00   0.00   88
 10  \w    -23.00  95.00   0.50   17.13    --    7.10  57.00  60.00  236
 11  \w    -47.00  35.00   0.50   17.13    --   -7.50 -82.00  60.00  164
 12  \w    -70.00 -40.00   0.50   17.13    --   -7.50 -77.00  30.00   60
 13  \w    -62.00 -14.00   0.50   17.13    --   -7.50 -82.00 -60.00   96
;
_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      0.0663244000
_diffrn_orient_matrix_UB_12      -0.0555304000
_diffrn_orient_matrix_UB_13      0.0189886000
_diffrn_orient_matrix_UB_21      0.0474345000
_diffrn_orient_matrix_UB_22      0.0434080000
_diffrn_orient_matrix_UB_23      -0.0045659000
_diffrn_orient_matrix_UB_31      -0.0362642000
_diffrn_orient_matrix_UB_32      0.0357890000
_diffrn_orient_matrix_UB_33      0.0278214000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31031
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.946
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58658
_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    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0532P)^2^+0.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6338
_reflns_number_total             7664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01769a2.cif
_cod_data_source_block           aj1999
_cod_database_code               7713975
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCoCl
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.865
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4(0.046) H2(0.051) H3(0.055) H13(0.058) H14(0.053) H12(0.057)
 H24(0.059) H7A(0.071) H7B(0.071) H7C(0.071) H19(0.056) H25(0.063) H28(0.058)
 H26(0.059) H9A(0.078) H9B(0.078) H9C(0.078) H31(0.066) H16(0.059) H21A(0.105)
 H21B(0.105) H21C(0.105) H20A(0.112) H20B(0.112) H20C(0.112) H30A(0.127)
 H30B(0.127) H30C(0.127) H17A(0.123) H17B(0.123) H17C(0.123) H18A(0.116)
 H18B(0.116) H18C(0.116) H29A(0.136) H29B(0.136) H29C(0.136) H32A(0.124)
 H32B(0.124) H32C(0.124) H33A(0.153) H33B(0.153) H33C(0.153) H1A(0.19) H1B(0.19)
 Fixed X: H4(0.437917) H2(0.188012) H3(0.298228) H13(0.691017) H14(0.409037)
 H12(0.889058) H24(-0.106643) H7A(0.576779) H7B(0.446385) H7C(0.631866)
 H19(0.811909) H25(0.022445) H28(0.455339) H26(0.257109) H9A(0.151662) H9B(-
 0.00068) H9C(0.048307) H31(0.032018) H16(0.233923) H21A(0.995026)
 H21B(1.008126) H21C(0.842589) H20A(0.96228) H20B(1.086893) H20C(1.062168)
 H30A(0.396899) H30B(0.513252) H30C(0.318172) H17A(0.1857) H17B(0.057459)
 H17C(0.233368) H18A(0.20219) H18B(0.037066) H18C(0.158021) H29A(0.582484)
 H29B(0.683435) H29C(0.568762) H32A(-0.173821) H32B(-0.128913) H32C(0.010266)
 H33A(-0.17079) H33B(-0.253545) H33C(-0.277135) H1A(0.646065) H1B(0.608028)
 Fixed Y: H4(0.196419) H2(0.343875) H3(0.158237) H13(0.793921) H14(0.866616)
 H12(0.626284) H24(1.192994) H7A(0.401612) H7B(0.336148) H7C(0.25851)
 H19(0.445367) H25(1.214135) H28(0.659199) H26(1.018084) H9A(0.542598)
 H9B(0.600825) H9C(0.714356) H31(0.875895) H16(0.745221) H21A(0.622901)
 H21B(0.521948) H21C(0.66506) H20A(0.310026) H20B(0.303861) H20C(0.410301)
 H30A(0.777624) H30B(0.611903) H30C(0.672519) H17A(0.765578) H17B(0.75151)
 H17C(0.618168) H18A(0.995418) H18B(0.981484) H18C(0.99852) H29A(0.826318)
 H29B(0.702085) H29C(0.863406) H32A(1.184673) H32B(1.077997) H32C(1.116194)
 H33A(0.854367) H33B(0.931451) H33C(1.02722) H1A(0.923558) H1B(0.953339)
 Fixed Z: H4(0.215849) H2(0.376138) H3(0.307443) H13(-0.02675) H14(-0.005779)
 H12(0.044541) H24(0.360269) H7A(0.086377) H7B(0.108751) H7C(0.135013)
 H19(0.189815) H25(0.449964) H28(0.433184) H26(0.492713) H9A(0.453059)
 H9B(0.404836) H9C(0.436539) H31(0.271425) H16(0.13216) H21A(0.163005)
 H21B(0.226931) H21C(0.209995) H20A(0.105609) H20B(0.159146) H20C(0.096093)
 H30A(0.553031) H30B(0.542063) H30C(0.531998) H17A(-0.001821) H17B(0.049508)
 H17C(0.043651) H18A(0.114803) H18B(0.096536) H18C(0.042646) H29A(0.404198)
 H29B(0.458179) H29C(0.475653) H32A(0.257657) H32B(0.202949) H32C(0.23165)
 H33A(0.340045) H33B(0.273289) H33C(0.330964) H1A(0.100589) H1B(0.163839)
;
_shelx_res_checksum              81960
_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 1.678
_oxdiff_exptl_absorpt_empirical_full_min 0.528