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_1547963
_publ_contact_author_name        'Alessandro Prescimone'
_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_absolute_configuration .
_chemical_compound_source        'F.J. Martinez Lillo'
_chemical_formula_moiety         'C6 H9 Cl4 N3 Re1'
_chemical_formula_sum            'C6 H9 Cl4 N3 Re'
_chemical_formula_weight         451.17
_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     'from the 2.6GPa structure'
_audit_creation_date             13-10-15
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.835(2)
_cell_length_b                   12.816(15)
_cell_length_c                   8.746(3)
_cell_measurement_reflns_used    1438
_cell_measurement_temperature    300
_cell_measurement_theta_max      18
_cell_measurement_theta_min      2.391
_cell_volume                     1102.4(14)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_pressure         4300000
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.475
_diffrn_measured_fraction_theta_max 0.447
_diffrn_measurement_device       'Rigaku Saturn 724 CCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type
'Synchrotron - Diamond Light Source Beamline I19'
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1894
_diffrn_reflns_theta_full        13.449
_diffrn_reflns_theta_max         17.696
_diffrn_reflns_theta_min         2.392
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.372
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_recrystallization_method
; 
evaporation of a CH3CN solution
;
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1071
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         400
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.0002364
_refine_ls_shift/su_mean         0.0000105
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.719 -0.964 0.923E-01 -0.362 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0599
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0508
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                400
_reflns_number_total             527
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0702
_oxford_refine_ls_scale          0.1164(7)
_oxford_reflns_number_all        483
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'recl04 in Pnma'
_cod_data_source_file            ReCl4MeCN.MeCN4.30GPa.cif
_cod_data_source_block           recl04
_cod_original_cell_volume        1102.4(13)
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C6 H9 Cl4 N3 Re1'
_cod_database_code               1547963
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT RE(1, U'S) 
CONT CL(2,U'S) UNTIL CL(4) 
CONT N(5,U[ISO]) UNTIL C(3) 
CONT C(2,U[ISO]) UNTIL C(1) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
DISTANCE 1.140000 , 0.050000 = N(2) TO C(1) 
DISTANCE 1.450000 , 0.050000 = C(2) TO C(1) 
DISTANCE 1.150000 , 0.050000 = N(5) TO C(6) 
DISTANCE 1.450000 , 0.050000 = C(6) TO C(3)
VIBR .0, 0.00500 = CL(4,3,1,0,1) TO N(5,3,1,0,1) 
VIBR .0, 0.00500 = CL(2) TO N(5,3,1,0,1) 
VIBR .0, 0.00500 = CL(2) TO CL(4,3,1,0,1) 
VIBR .0, 0.00500 = CL(3) TO N(5,3,1,0,1) 
VIBR .0, 0.00500 = CL(3) TO CL(4,3,1,0,1) 
VIBR .0, 0.00500 = CL(3) TO CL(2) 
VIBR .0, 0.00500 = CL(4) TO N(5,3,1,0,1) 
VIBR .0, 0.00500 = CL(4) TO CL(4,3,1,0,1) 
VIBR .0, 0.00500 = CL(4) TO CL(2) 
VIBR .0, 0.00500 = CL(4) TO CL(3) 
VIBR .0, 0.00500 = N(5) TO N(5,3,1,0,1) 
VIBR .0, 0.00500 = N(5) TO CL(4,3,1,0,1) 
VIBR .0, 0.00500 = N(5) TO CL(2) 
VIBR .0, 0.00500 = N(5) TO CL(3) 
VIBR .0, 0.00500 = N(5) TO CL(4) 
VIBR .0, 0.00200 = N(5) TO C(6) 
VIBR .0, 0.00200 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(3) TO N(5) 
VIBR .0, 0.00200 = C(2) TO C(1,3,1,0,1) 
VIBR .0, 0.00200 = C(2) TO C(1) 
VIBR .0, 0.00500 = C(1) TO C(1,3,1,0,1) 
VIBR .0, 0.00200 = N(2) TO N(2,-1,1,1,1,1) 
VIBR .0, 0.00200 = N(2) TO C(1) 
VIBR .0, 0.00500 = C(1) TO N(2,-1,1,1,1,1) 
VIBR .0, 0.00500 = N(2) TO C(2) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(5) TO C(6) 
U(IJ) .0, 0.08000 = C(6) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(1,3,1,0,1) 
U(IJ) .0, 0.04000 = C(2) TO C(1) 
U(IJ) .0, 0.04000 = N(2) TO N(2,-1,1,1,1,1) 
U(IJ) .0, 0.04000 = N(2) TO C(1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;