Pressure induced enhancement of the magnetic ordering temperature in rhenium(IV) monomers
Christopher H. Woodall; Gavin A. Craig; Alessandro Prescimone; Martin Misek; Joan Cano; Juan Faus; Michael R. Probert; Simon Parsons; Stephen Moggach; Jose Martinez-Lillo; Mark Murrie; Konstantin V. Kamenev; Euan K. Brechin; Nature Communications 7 (2017) 13870–; doi:10.1038/ncomms13870

data_1547951
_publ_section_title
;
 Pressure induced enhancement of the magnetic ordering temperature in
 rhenium(IV) monomers
;
_journal_name_full               'Nature Communications'
_journal_page_first              13870
_journal_paper_doi               10.1038/ncomms13870
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C8 H6 Br4 N4 Re'
_chemical_formula_sum            'C8 H6 Br4 N4 Re'
_chemical_formula_weight         664.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2129(5)
_cell_length_b                   10.5779(5)
_cell_length_c                   13.0532(6)
_cell_measurement_reflns_used    4774
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.48
_cell_volume                     1272.08(11)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.670
_diffrn_measured_fraction_theta_max 0.627
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.670
_diffrn_reflns_Laue_measured_fraction_max 0.627
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7464
_diffrn_reflns_point_group_measured_fraction_full 0.671
_diffrn_reflns_point_group_measured_fraction_max 0.625
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.795
_diffrn_reflns_theta_min         2.478
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.097
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0773 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.7066.
The \l/2 correction factor is 0.0015.

PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low....... 0.667 Note
COMMENT... Low completeness due to limited access to reciprocal space due to
masking by high pressure cell
  
PLAT201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s)...... 12 Report
COMMENT...Carbon and Nitrogen atoms were refined isotropically to keep their
treament consistent across refinements. All other non-hydrogen atoms were refined 
anisotropically

PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.0200 Ang.
COMMENT...No Comment
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.467
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details
;
 Flack x determined using 650 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0190P)^2^+17.3217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_full    0.672
_reflns_Friedel_fraction_max     0.623
_reflns_number_gt                1633
_reflns_number_total             1707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ReBr4bpym1.06GPa.cif
_cod_data_source_block           chw007
_cod_database_code               1547951
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(N3) = Uiso(N4)
Uiso(N1) = Uiso(N2)
Uiso(C8) = Uiso(C3)
Uiso(C5) = Uiso(C2)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
;
_shelx_res_checksum              67499
_shelx_hkl_checksum              40021
_olex2_submission_special_instructions 'No special instructions were received'