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_1576540
_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         'C70 H68 Cl6 Cu2 N6 O4, 3(C H Cl3)'
_chemical_formula_sum            'C73 H71 Cl15 Cu2 N6 O4'
_chemical_formula_weight         1755.18
_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   mixed
_audit_creation_date             2014-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.96470(10)
_cell_length_b                   19.2212(3)
_cell_length_c                   19.3245(3)
_cell_measurement_temperature    133(2)
_cell_volume                     3928.98(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24604
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         2.718
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+6.9342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7810
_reflns_number_total             8937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fo4112.cif
_cod_data_source_block           fo4112
_cod_database_code               1576540
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.937
_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. Others
 Fixed Sof: Cl32(0.5) Cl33(0.5) C3C(0.5) Cl31(0.5) H3C(0.5) Cl42(0.5)
 Cl41(0.5) Cl43(0.5) C4C(0.5) H4C(0.5) Cl21(0.5) Cl22(0.5) Cl23(0.5) C2C(0.5)
 H2C(0.5)
3.a Free rotating group:
 C23(C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,Cl12,Cl13,Cl11,C1C,Cl32,Cl33,
 C3C,Cl31,H3C,Cl42,Cl41,Cl43,C4C,H4C), Cl21(Cl22,Cl23,C2C,H2)
3.b Ternary CH refined with riding coordinates:
 C2C(H2C)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2A), C3(H3A), C4(H4), C5(H5), C7(H7), C9(H9), C13(H13), C17(H17),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25)
3.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              86714
_shelx_hkl_checksum              32580