Experimental determination of spin-dependent electron density by joint refinement of X-ray and polarized neutron diffraction data
Deutsch, Maxime; Claiser, Nicolas; Pillet, Sébastien; Chumakov, Yurii; Becker, Pierre; Gillet, Jean-Michel; Gillon, Béatrice; Lecomte, Claude; Souhassou, Mohamed; Acta Crystallographica Section A 68 (2012) 675–686; doi:10.1107/S0108767312031996

data_2310008
_publ_section_title
;
 Experimental determination of spin-dependent electron density by joint
 refinement of X-ray and polarized neutron diffraction data
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              675
_journal_page_last               686
_journal_paper_doi               10.1107/S0108767312031996
_journal_volume                  68
_journal_year                    2012
_chemical_formula_sum            'C7 H16 Cu Mn N2 O11'
_chemical_formula_weight         422.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7158(3)
_cell_length_b                   21.3520(5)
_cell_length_c                   5.1745(2)
_cell_measurement_temperature    10(5)
_cell_volume                     1404.92(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      10(5)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8505
_diffrn_reflns_theta_full        53.34
_diffrn_reflns_theta_max         53.34
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    2.483
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
;
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.2673
_exptl_crystal_size_mid          0.1561
_exptl_crystal_size_min          0.0620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         8505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0290
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+1.3214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                6880
_reflns_number_total             8505
_reflns_threshold_expression     >3\s(I)
_cod_data_source_file            wl5162.cif
_cod_data_source_block           I
_cod_database_code               2310008