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_1576539
_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         'C100 H130 Cu2 N6 O4, 4(C H Cl3)'
_chemical_formula_sum            'C104 H134 Cl12 Cu2 N6 O4'
_chemical_formula_weight         2084.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 92.768(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3077(5)
_cell_length_b                   17.8055(7)
_cell_length_c                   25.9654(9)
_cell_measurement_temperature    133(2)
_cell_volume                     5683.5(4)
_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 0.881
_diffrn_measured_fraction_theta_max 0.857
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.881
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21272
_diffrn_reflns_point_group_measured_fraction_full 0.881
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         1.570
_exptl_absorpt_coefficient_mu    0.705
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         11176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1310P)^2^+19.8706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2364
_refine_ls_wR_factor_ref         0.2473
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9354
_reflns_number_total             11176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fo4111.cif
_cod_data_source_block           fo4111
_cod_database_code               1576539
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H2CA(0.5) H2C(0.5) Cl21(0.5) Cl32(0.5) Cl22(0.5) Cl33(0.5)
 Cl23(0.5) Cl31(0.5)
3.a Ternary CH refined with riding coordinates:
 C1C(H1C), C2C(H2CA), C2C(H2C)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C24(H24), C22(H22), C20(H20), C17(H17), C19(H19), C9(H9), C13(H13),
 C7(H7), C5(H5), C3(H3A)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              58620
_shelx_hkl_checksum              6792