Experimental and theoretical investigations on transition metal and lanthanide containing molecular magnets
Hornig, David; Dissertation Friedrich Schiller University Jena 2015 (2015) 1–183; doi:10.22032/dbt.25623

data_1576543
_publ_contact_author_name
;
;
_publ_section_title
;
 Experimental and theoretical investigations on transition metal and
 lanthanide containing molecular magnets
;
_journal_name_full
'Dissertation Friedrich Schiller University Jena'
_journal_page_first              1
_journal_page_last               183
_journal_paper_doi               10.22032/dbt.25623
_journal_volume                  2015
_journal_year                    2015
_chemical_formula_moiety         'C68 H66 Co2 N6 O4'
_chemical_formula_sum            'C68 H66 Co2 N6 O4'
_chemical_formula_weight         1149.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8924(3)
_cell_length_b                   23.0517(4)
_cell_length_c                   18.0297(3)
_cell_measurement_temperature    133(2)
_cell_volume                     6602.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22594
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         1.901
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0895P)^2^+8.3588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6050
_reflns_number_total             7573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fo4385.cif
_cod_data_source_block           fo4385
_cod_database_code               1576543
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), N3(H3), C13(H13), C19(H19), C7(H7), C17(H17), C4(H4), C20(H20),
 C22(H22), C2(H2), C3(H3A), C24(H24), C25(H25), C23(H23), C5(H5)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              95091
_shelx_hkl_checksum              9722