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_1547959
_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 ambient pressure structure'
_audit_creation_date             13-10-14
_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                   10.2971(5)
_cell_length_b                   13.4016(9)
_cell_length_c                   9.6238(10)
_cell_measurement_reflns_used    6258
_cell_measurement_temperature    300
_cell_measurement_theta_max      20.275
_cell_measurement_theta_min      2.237
_cell_volume                     1328.06(18)
_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         300000
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.719
_diffrn_measured_fraction_theta_max 0.694
_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  0.044
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11196
_diffrn_reflns_theta_full        15.454
_diffrn_reflns_theta_max         20.334
_diffrn_reflns_theta_min         1.781
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.629
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.256
_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          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.84
_refine_diff_density_min         -1.53
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9141
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1315
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.0009936
_refine_ls_shift/su_mean         0.0000439
_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: 
 0.151 -0.109E-01 -0.232E-01 -0.717E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0275
_refine_ls_wR_factor_gt          0.0222
_refine_ls_wR_factor_ref         0.0222
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1315
_reflns_number_total             1470
_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   0.0257
_oxford_refine_ls_scale          0.12197(15)
_oxford_reflns_number_all        1459
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'recl06a in Pnma'
_cod_data_source_file            ReCl4MeCN.MeCN0.30GPa.cif
_cod_data_source_block           recl06a
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C6 H9 Cl4 N3 Re1'
_cod_database_code               1547959
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT RE(1, U'S) 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) 
DISTANCE 1.140000 , 0.050000 = N(2) TO C(1) 
DISTANCE 1.450000 , 0.050000 = C(2) TO C(1) 
ANGLE 179.000000 , 5.000000 = C(2) TO C(1) TO N(2) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
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                                                                             
;