Inorganic co-crystal formation and thermal disproportionation in a dicyanometallate ‘superperovskite’
Hill, Joshua A.; Murray, Claire A.; Tang, Chiu C.; Thygesen, Peter M. M.; Thompson, Amber L.; Goodwin, Andrew L.; Chemical Communications  (2019) –; doi:10.1039/C8CC10277E

data_7123329
_publ_section_title
;
 Inorganic co-crystal formation and thermal disproportionation in a
 dicyanometallate &#x2018;superperovskite&#x2019;
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10277E
_journal_year                    2019
_chemical_formula_moiety         'C38 H72 Au3 Cl1.00 Mn1 N8 O4.00'
_chemical_formula_sum            'C38 H72 Au3 Cl Mn N8 O4'
_chemical_formula_weight         1386.32
_chemical_name_systematic
;
(bis)tetra(n-butyl)ammonium manganese(II) (tris)dicyanoaurate perchlorate
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_block_doi                 10.5517/ccdc.csd.cc2240t2
_audit_creation_date             2018-12-29
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4048(3)
_cell_length_b                   21.4048(2)
_cell_length_c                   21.3901(2)
_cell_measurement_reflns_used    37078
_cell_measurement_temperature    30
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     9800.21(19)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      30
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8625
_diffrn_reflns_theta_full        25.370
_diffrn_reflns_theta_max         32.114
_diffrn_reflns_theta_min         1.844
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.538
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5335.992
_exptl_crystal_recrystallization_method 'Solution diffusion'
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         9.96
_refine_diff_density_min         -15.97
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0653
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4677
_refine_ls_number_restraints     629
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.1286
_refine_ls_shift/su_max          0.0059366
_refine_ls_shift/su_mean         0.0008734
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F) + ( 0.00P)^2^ + 2.89P] 
 ,where P=(max(Fo,0) + 2Fc)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2779
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.1662
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                5488
_reflns_number_total             8625
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.04
_oxford_diffrn_Wilson_scale      4.74
_oxford_refine_ls_r_factor_ref   0.1142
_oxford_refine_ls_scale          0.64(5)
_oxford_reflns_number_all        8625
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 048jah14-
_cod_data_source_file            c8cc10277e2.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        9800.2(2)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C38 H72 Au3 Cl1.00 Mn1 N8 O4.00'
_cod_database_code               7123329