Stereochemistry of coordination polyhedra vs. single ion magnetism in penta- and hexacoordinated Co(ii) complexes with tridentate rigid ligands.
Brachňaková, Barbora; Matejová, Simona; Moncol, Ján; Herchel, Radovan; Pavlik, Ján; Moreno-Pineda, Eufemio; Ruben, Mario; Šalitroš, Ivan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1249–1264; doi:10.1039/c9dt04592a

data_7702992
_publ_section_title
;
 Stereochemistry of coordination polyhedra vs. single ion magnetism in
 penta- and hexacoordinated Co(ii) complexes with tridentate rigid
 ligands.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1249
_journal_page_last               1264
_journal_paper_doi               10.1039/c9dt04592a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C49 H57 Br2 Co N5'
_chemical_formula_sum            'C49 H57 Br2 Co N5'
_chemical_formula_weight         934.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-18 deposited with the CCDC.	2019-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.413(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9513(4)
_cell_length_b                   8.8923(2)
_cell_length_c                   30.3407(7)
_cell_measurement_reflns_used    40285
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.89
_cell_measurement_theta_min      2.94
_cell_volume                     4802.76(19)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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_temperature      100
_diffrn_detector                 'Pilatus3R 300K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS3R 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            58225
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.409
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.023
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'STOE LANA, J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0254P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5142
_reflns_number_total             9211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04592a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7702990--7702993.cif.'
_cod_original_cell_volume        4802.75(19)
_cod_database_code               7702992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.419
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C28A \\sim C27-C28B \\sim C27-C29A \\sim C27-C29B \\sim C27-C30A \\sim
C27-C30B
 with sigma of 0.02
 C31-C32A \\sim C31-C33A \\sim C31-C34A \\sim C31-C32B \\sim C31-C33B \\sim
C31-C34B
 with sigma of 0.02
 C42-C43A \\sim C42-C44A \\sim C42-C45A \\sim C42-C43B \\sim C42-C44B \\sim
C42-C45B
 with sigma of 0.02
 C46-C47A \\sim C46-C48A \\sim C46-C49A \\sim C46-C47B \\sim C46-C48B \\sim
C46-C49B
 with sigma of 0.02
 C28A-C29A \\sim C28A-C30A \\sim C29A-C30A \\sim C28B-C29B \\sim C28B-C30B
\\sim C29B-C30B
 with sigma of 0.02
 C32A-C33A \\sim C32A-C34A \\sim C33A-C34A \\sim C32B-C33B \\sim C32B-C34B
\\sim C33B-C34B
 with sigma of 0.02
 C43A-C44A \\sim C43A-C45A \\sim C44A-C45A \\sim C43B-C44B \\sim C43B-C45B
\\sim C44B-C45B
 with sigma of 0.02
 C47A-C48A \\sim C47A-C49A \\sim C48A-C49A \\sim C47B-C48B \\sim C47B-C49B
\\sim C48B-C49B
 with sigma of 0.02
 C23-C28A \\sim C23-C29A \\sim C23-C30A \\sim C23-C28B \\sim C23-C29B \\sim
C23-C30B
 with sigma of 0.02
 C25-C32A \\sim C25-C33A \\sim C25-C34A \\sim C25-C32B \\sim C25-C33B \\sim
C25-C34B
 with sigma of 0.02
 C38-C43A \\sim C38-C44A \\sim C38-C45A \\sim C38-C43B \\sim C38-C44B \\sim
C38-C45B
 with sigma of 0.02
 C40-C47A \\sim C40-C48A \\sim C40-C49A \\sim C40-C47B \\sim C40-C48B \\sim
C40-C49B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28A) = Uanis(C28B)
Uanis(C29A) = Uanis(C29B)
Uanis(C30A) = Uanis(C30B)
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
Uanis(C34A) = Uanis(C34B)
Uanis(C43A) = Uanis(C43B)
Uanis(C44A) = Uanis(C44B)
Uanis(C45A) = Uanis(C45B)
Uanis(C47A) = Uanis(C47B)
Uanis(C48A) = Uanis(C48B)
Uanis(C49A) = Uanis(C49B)
4. Rigid body (RIGU) restrains
 C28A, C29A, C30A, C28B, C29B, C30B, C32A, C33A, C34A, C32B, C33B, C34B, C43A,
 C44A, C45A, C43B, C44B, C45B, C47A, C48A, C49A, C47B, C48B, C49B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(2)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(2)
 Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44B)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(3)
 Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44A)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(3)
 Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48B)=Sof(H48D)=Sof(H48E)=
 Sof(H48F)=Sof(C49B)=Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(4)
 Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48A)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C35(H35A,H35B)
6.b Me refined with riding coordinates:
 C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C28B(H28D,
 H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C32A(H32A,H32B,H32C),
 C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C32B(H32D,H32E,H32F), C33B(H33D,
 H33E,H33F), C34B(H34D,H34E,H34F), C43A(H43A,H43B,H43C), C44A(H44A,H44B,H44C),
 C45A(H45A,H45B,H45C), C43B(H43D,H43E,H43F), C44B(H44D,H44E,H44F), C45B(H45D,
 H45E,H45F), C47A(H47A,H47B,H47C), C48A(H48A,H48B,H48C), C49A(H49A,H49B,H49C),
 C47B(H47D,H47E,H47F), C48B(H48D,H48E,H48F), C49B(H49D,H49E,H49F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C22(H22), C24(H24), C26(H26), C37(H37), C39(H39),
  C41(H41)
;
_shelx_res_checksum              94684
_shelx_fab_checksum              68738
_olex2_submission_special_instructions 'No special instructions were received'