Indirect effect of hydrogen bonds on the magnetic coupling on Mn(iii) dinuclear compounds
Pagès, J. M.; Escriche-Tur, L.; Font-Bardia, M.; Aullón, G.; Corbella, M.; CrystEngComm 20 (2018) 6629–; doi:10.1039/C8CE01194J

data_7231566
_publ_section_title
;
 Indirect effect of hydrogen bonds on the magnetic coupling on Mn(iii)
 dinuclear compounds
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              6629
_journal_paper_doi               10.1039/C8CE01194J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C34 H24 Cl4 Mn2 N5 O9, N O3, C2 N, H2 O'
_chemical_formula_sum            'C36 H26 Cl4 Mn2 N7 O13'
_chemical_formula_weight         1016.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-05-09 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6545(12)
_cell_length_b                   14.0357(8)
_cell_length_c                   15.6154(10)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.54
_cell_volume                     4088.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17365
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.189
_diffrn_reflns_theta_min         2.544
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       prism
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.153
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.

'You can solve the structure taking into account two differents symetries ( the major symmetry or the minory symmetry group, respectively, Pbcn and Pca21). 
In our case (two probable groups were suggested, Pbcn and Pbca21) tne group with a major symmetry Pbcn was suggested and the refinement in this space group also proved to be reasonable with a high site symmetry. 
However, the R factor was higher [R = 0.22 and wR(F2) = 0.59] and the displacement elliposoid were elongated in a direction perpendicular to the crystallographic mirror axis. In the other hand, the resolution of the structure
with a minor simmetry group, Pca21, takes good values for the R factor [R = 0.07 and wR(F2) = 0.19] and yield chemically reasonable with the structure. An output of an statistical analysis of the current data set is shown.
Pca21 \`e c perpendicular a. \`e  0kl \`e l = 2n+1
               a perpedincular b. \`e k0l \`e k = 2n+1
Pbcn \`e h+k=2n+1 \`e No extinctions observed'

;
_refine_ls_abs_structure_Flack   0.19(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7592
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0735P)^2^+24.8109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                7067
_reflns_number_total             7592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01194j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7231565--7231566.cif.'
_cod_database_code               7231566
_shelxl_version_number           2014-1
_shelx_res_checksum              35421