Synthesis, structural and magnetic properties of cobalt(ii) complexes with pyridine-based macrocyclic ligand containing two pyridine pendant arms
Zahradníková, Eva; Pichon, Céline; Duhayon, Carine; Sutter, Jean-Pascal; Halaš, Petr; Drahoš, Bohuslav; RSC Advances 14 (2024) 28138–28147; doi:10.1039/D4RA02387K

data_7249286
_publ_section_title
;
 Synthesis, structural and magnetic properties of cobalt(ii) complexes
 with pyridine-based macrocyclic ligand containing two pyridine pendant
 arms
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              28138
_journal_page_last               28147
_journal_paper_doi               10.1039/D4RA02387K
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H35 Co N7 O2 S2  '
_chemical_formula_sum            'C29 H35 Co N7 O2 S2'
_chemical_formula_weight         636.71
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2024-07-17 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.20980(10)
_cell_length_b                   32.9484(3)
_cell_length_c                   9.78030(10)
_cell_measurement_reflns_used    22492
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.74
_cell_measurement_theta_min      2.68
_cell_volume                     2967.81(5)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2021) 
;
_computing_data_collection
; 
 'XtaLAB Synergy, Dualflex,HyPix, (Rigaku, 2021) 
;
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2021) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     2.256
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30483
_diffrn_reflns_theta_full        80.17
_diffrn_reflns_theta_max         73.823
_diffrn_reflns_theta_min         2.682
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.171
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 2157 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   -0.0264(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9526
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5758
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.0020007
_refine_ls_shift/su_mean         0.0000788
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 1.45P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0733
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0733
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_gt                5642
_reflns_number_total             6088
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.75
_oxford_diffrn_Wilson_scale      0.29
_oxford_refine_ls_scale          2.106(10)
_cod_data_source_file            d4ra02387k2.cif
_cod_data_source_block           20240708-CP-EZ9
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_Hall     'P 2c -2n '
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C29 H35 Co N7 O2 S2  '
_cod_database_code               7249286
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0274
_reflns_number_all               5758
_oxford_hooft_y                  -0.(0)
_oxford_bijvoet_difference       -0.0264(12)
_oxford_refined_flack_x          -0.0227(19)