Formation of the layered conductive magnet CrCl2(pyrazine)2 through redox-active coordination chemistry
Kasper S. Pedersen; Panagiota Perlepe; Michael L. Aubrey; Daniel N. Woodruff; Sebastian E. Reyes-Lillo; Anders Reinholdt; Laura Voigt; Zheshen Li; Kasper Borup; Mathieu Rouzieres; Dumitru Samohvalov; Fabrice Wilhelm; Andrei Rogalev; Jeffrey B. Neaton; Jeffrey R. Long; Rodolphe Clerac; Nature Chemistry 10 (2018) 1056–1061; doi:10.1038/s41557-018-0107-7

data_1551499
_publ_section_title
;
 Formation of the layered conductive magnet CrCl2(pyrazine)2 through
 redox-active coordination chemistry
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1056
_journal_page_last               1061
_journal_paper_doi               10.1038/s41557-018-0107-7
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'C20 H20 Cl2 Cr N4, 0.25(H2 O), Cl O4'
_chemical_formula_sum            'C20 H20.5 Cl3 Cr N4 O4.25'
_chemical_formula_weight         543.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 93.2000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4559(3)
_cell_length_b                   15.1420(4)
_cell_length_c                   23.1601(6)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.647
_cell_measurement_theta_min      3.036
_cell_volume                     4711.5(2)
_computing_cell_refinement
'SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.704
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    5.003
_exptl_absorpt_correction_T_max  0.3108
_exptl_absorpt_correction_T_min  0.1866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1084 before and 0.0612 after correction. The Ratio of minimum to maximum transmission is 0.6004. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00444(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+2.0871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10272
_reflns_number_total             10810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_107_MOESM3_ESM.cif
_cod_data_source_block           dolle08
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C20 H20.50 Cl3 Cr N4 O4.25'
_cod_database_code               1551499
_shelx_estimated_absorpt_t_max   0.609
_shelx_estimated_absorpt_t_min   0.434
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(Cl1G)=Sof(O1G)=Sof(O3G)=1-FVAR(1)
 Sof(Cl1D)=Sof(O1D)=Sof(O3D)=FVAR(1)
 Sof(Cl1F)=Sof(O2F)=Sof(O4F)=1-FVAR(2)
 Sof(Cl1C)=Sof(O2C)=Sof(O4C)=FVAR(2)
 Fixed Sof: O1E(0.5) H1EA(0.5) H1EB(0.5)
3.a Riding coordinates:
 O1E(H1EA,H1EB)
3.b Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B),
 C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C13B(H13B), C14B(H14B),
  C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B),
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A),
  C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A)
;
_shelx_res_checksum              89233
_shelx_hkl_checksum              92760