Diazine based ligand supported CoII3 and CoII4 coordination complexes: role of anions
Sikdar, Yeasin; Goswami, Ranadip; Modak, Ritwik; Basak, Megha; Heras Ojea, María José; Murrie, Mark; Goswami, Sanchita; New Journal of Chemistry 42 (2018) 17587–; doi:10.1039/C8NJ02955E

data_7057739
_publ_section_title
;
 Diazine based ligand supported CoII3 and CoII4 coordination complexes:
 role of anions
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17587
_journal_paper_doi               10.1039/C8NJ02955E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C50 H50 Co4 N8 O20'
_chemical_formula_sum            'C50 H50 Co4 N8 O20'
_chemical_formula_weight         1318.70
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-28 deposited with the CCDC.
2018-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.743(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6970(8)
_cell_length_b                   19.1711(10)
_cell_length_c                   18.4094(10)
_cell_measurement_reflns_used    88121
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.8
_cell_volume                     5460.0(5)
_computing_cell_refinement       'BRUKER APEX III'
_computing_data_collection       'BRUKER APEX III'
_computing_data_reduction        'SAINT (BRUKER APEX III)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST ECO'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88121
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         2.840
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(SHELDRICK,2008)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Solvent diffusion'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00097(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         13570
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0428P)^2^+5.4632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9941
_reflns_number_total             13570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02955e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7057739--7057743.cif.'
_cod_database_code               7057739
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O18A-N8 \\sim O18B-N8 \\sim O19B-N8 \\sim O19A-N8
 with sigma of 0.02
3. Others
 Fixed Sof: H14(0.5) H14A(0.5) O18A(0.5) O18B(0.5) O19A(0.5) O19B(0.5)
4.a Riding coordinates:
 O13(H13), O14(H14,H14A)
4.b Me refined with riding coordinates:
 C50(H50A,H50B,H50C)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13A),
 C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              73500
_shelx_hkl_checksum              98917
_olex2_submission_special_instructions 'No special instructions were received'