Colossal thermal expansion and negative thermal expansion in simple halogen bonded complexes
Jones, Richard H.; Knight, Kevin S.; Marshall, William G.; Clews, John; Darton, Richard J.; Pyatt, Daniel; Coles, Simon J.; Horton, Peter N.; CrystEngComm 16 (2014) 237–; doi:10.1039/c3ce41909f

data_7213567
_publ_section_title
;
 Colossal thermal expansion and negative thermal expansion in simple
 halogen bonded complexes
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              237
_journal_paper_doi               10.1039/c3ce41909f
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C5 H5 Br1 I1 N1'
_chemical_formula_sum            'C5 H5 Br I N'
_chemical_formula_weight         285.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 98.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.25640(10)
_cell_length_b                   12.7251(4)
_cell_length_c                   13.9443(3)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    110
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     747.25(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8362
_diffrn_reflns_theta_full        27.522
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         3.359
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.534
_exptl_absorpt_correction_T_max  0.08
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.81
_refine_diff_density_min         -1.17
_refine_ls_extinction_coef       28.9(17)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9808
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1720
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.0006887
_refine_ls_shift/su_mean         0.0000370
_refine_ls_structure_factor_coef Fsqd
_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: 
 31.4 47.6 26.5 7.94 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0647
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0647
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1636
_reflns_number_total             1722
_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   0.0267
_oxford_refine_ls_scale          0.4083(8)
_oxford_reflns_number_all        1720
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3ce41909f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C5 H5 Br1 I1 N1'
_cod_database_code               7213567
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT I    (    1 ,X'S,U'S)  UNTIL C    (    6 ) 
CONT H    (    2 ,X'S,U[ISO])  UNTIL H    (    6 ) 
CONT EXTPARAM 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;