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_7702993
_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         'C98 H114 Co N10, 2(C H4 O), 2(Br), H2 O'
_chemical_formula_sum            'C100 H124 Br2 Co N10 O3'
_chemical_formula_weight         1732.83
_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             2019-09-18
_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                67.463(2)
_cell_angle_beta                 87.059(2)
_cell_angle_gamma                72.737(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5981(4)
_cell_length_b                   18.2954(5)
_cell_length_c                   21.4975(6)
_cell_measurement_reflns_used    90336
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.67
_cell_measurement_theta_min      2.23
_cell_volume                     4705.4(2)
_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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_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 0.988
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari with Xenocs Genix3D Cu HF'
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            117780
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.529
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  0.421
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   X-AREA
_exptl_crystal_colour            'yellowish orange'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         17704
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13322
_reflns_number_total             17704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04592a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7702990--7702993.cif.'
_cod_database_code               7702993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.362
_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, All O(H) groups
2. Restrained distances
 C95-C96 \\sim C95-C97 \\sim C95-C98 \\sim C95-C96A \\sim C95-C97A \\sim
C95-C98A
 with sigma of 0.02
 C96-C97 \\sim C96-C98 \\sim C97-C98 \\sim C96A-C97A \\sim C96A-C98A \\sim
C97A-C98A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C96) = Uanis(C96A)
Uanis(C97) = Uanis(C97A)
Uanis(C98) = Uanis(C98A)
4. Rigid body (RIGU) restrains
 C96, C97, C98, C96A, C97A, C98A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C96A)=Sof(H96D)=Sof(H96E)=Sof(H96F)=Sof(C97A)=Sof(H97D)=Sof(H97E)=
 Sof(H97F)=Sof(C98A)=Sof(H98D)=Sof(H98E)=Sof(H98F)=1-FVAR(1)
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C54(H54A,H54B), C69(H69A,H69B), C80(H80A,H80B)
6.b Me refined with riding coordinates:
 C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C96A(H96D,H96E,
 H96F), C97A(H97D,H97E,H97F), C98A(H98D,H98E,H98F)
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), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C41(H41),
 C43(H43), C45(H45), C56(H56), C58(H58), C60(H60), C71(H71), C73(H73), C75(H75),
  C82(H82), C84(H84), C86(H86)
6.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C100(H10A,H10B,H10C),
 C99(H99A,H99B,H99C)
6.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O1(H1)
;
_shelx_res_checksum              94787
_shelx_fab_checksum              10232
_olex2_submission_special_instructions 'No special instructions were received'