Enhanced relative stability of heterobimetallic Fe(II), Zn(II), and Mg(II) clusters supported by a µ-phenoxo bridge
Kerber, William D.; Hartnett, D. Sean; Wang, Aiqiu; Mafrice, Carson Hawkins; Siegler, Maxime A.; Inorganica Chimica Acta 506 (2020) 119547–; doi:10.1016/j.ica.2020.119547

data_1565170
_publ_section_title
;
 Enhanced relative stability of heterobimetallic Fe(II), Zn(II), and
 Mg(II) clusters supported by a &#x00B5;-phenoxo bridge
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119547
_journal_paper_doi               10.1016/j.ica.2020.119547
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety
'2(C16 H22 F Mg2 N2 O13), H12 Mg O6, 14(H2 O)'
_chemical_formula_sum            'C32 H84 F2 Mg5 N4 O46'
_chemical_formula_weight         1420.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                92.844(2)
_cell_angle_beta                 113.681(3)
_cell_angle_gamma                90.617(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8336(3)
_cell_length_b                   11.3855(3)
_cell_length_c                   13.3069(4)
_cell_measurement_reflns_used    12221
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      11.77
_cell_volume                     1500.45(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16068
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.872
_diffrn_reflns_theta_min         3.633
_diffrn_standards_decay_%        .
_diffrn_standards_interval_time  .
_diffrn_standards_number         .
_exptl_absorpt_coefficient_mu    1.776
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8695
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7952
_reflns_number_total             8695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Kerber_1293_Structure1.cif
_cod_data_source_block           1
_cod_database_code               1565170
_shelx_shelxl_version_number     2014/7
_twin_information
;

 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (38.43 (release 21-03-2016)) * * *
Laue class: 1bar - Friedel mate is equivalent
Lattice type: P-lattice 
DC PROFFITRRPTWIN INFO: Step 1 - Loading orientation matrices (UB) of 2 components
 
DC PROFFITRRPTWIN INFO: Loading UB component 1
 
DC PROFFITRRPTWIN INFO: Loading UB component 2
 
DC PROFFITRRPTWIN INFO: Step 2 - Computing crossed twin laws
 
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (  10.830   11.387   13.299    92.84   113.67    90.61)
Matrix 2 is taken from component 2 (  10.859   11.405   13.303    93.42   114.01    90.28)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:   0.9909  -0.0070  -0.0126    -0.0026   0.9979  -0.0063     0.0271   0.0201   1.0094   det 0.998544
TL-1=UB[2]*UB[1]-1:   1.0089   0.0069   0.0127     0.0024   1.0020   0.0063    -0.0271  -0.0202   0.9902   det 1.001458
Rot= 1.4988 deg around the following vectors: 
Reciprocal space (hkl): 0.6081 -0.7923 -0.0493
Direct space (uvw)    : 0.6868 -0.7088 0.1613
 
DC PROFFITRRPTWIN INFO: Step 3 - Loading reflections of 2 components
 
DC PROFFITRRPTWIN ALL INFO: Component 1
DC PROFFITRRPTWIN INFO: Face list of component 1 
  1:  -1.5307  -6.9078  -0.9665  d=   0.0682
  2:  -6.7756   1.4784   4.7299  d=   0.1300
  3:  -5.1865   4.5548   4.5825  d=   0.1267
  4:   5.1402   4.9048  -1.8948  d=   0.0884
  5:   5.1487  -4.5866   0.0899  d=   0.1196
  6:   1.2218  -2.5064   6.8569  d=   0.0887
  7:  -5.1515   3.2183   6.5184  d=   0.1301
  8:  -5.3842   4.5982   0.8614  d=   0.1305
  9:   1.0440   0.8001  -8.3225  d=   0.0917
 10:   4.9985   2.9994   2.0003  d=   0.0887
 11:   6.9989  -0.9985  -1.9985  d=   0.1200
 12:  -0.9988  -4.9978  -4.9990  d=   0.0898
 13:  -1.9996  -6.0000   4.9980  d=   0.1186
 14:   3.9996   4.0012  -6.9972  d=   0.0959
 15:   1.9996   6.0000  -4.9980  d=   0.1051
 16:   5.9995   1.0021  -6.9971  d=   0.1298
 17:   0.0010  -0.9979  -7.9978  d=   0.0831
 18:   2.0002   3.0014  -7.9973  d=   0.0926
 19:   2.9996  -5.9990   2.9993  d=   0.1157
 20:   2.9987  -0.0011   5.9988  d=   0.0953
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:  -1.6039  -6.9313  -0.7761  d=   0.0682
  2:  -6.7658   1.4948   4.8375  d=   0.1300
  3:  -5.1433   4.5802   4.5864  d=   0.1267
  4:   5.1955   4.9150  -2.1146  d=   0.0884
  5:   5.1642  -4.5827   0.0420  d=   0.1196
  6:   1.3025  -2.4650   6.8073  d=   0.0887
  7:  -5.0926   3.2534   6.5294  d=   0.1301
  8:  -5.3896   4.5997   0.9062  d=   0.1305
  9:   0.9533   0.7515  -8.2856  d=   0.0917
 10:   5.0888   3.0301   1.7847  d=   0.0887
 11:   7.0289  -0.9962  -2.1485  d=   0.1200
 12:  -1.1053  -5.0417  -4.8222  d=   0.0898
 13:  -1.9951  -5.9851   5.1244  d=   0.1186
 14:   3.9739   3.9745  -7.1180  d=   0.0959
 15:   1.9951   5.9851  -5.1244  d=   0.1051
 16:   5.9710   0.9743  -7.1115  d=   0.1298
 17:  -0.1072  -1.0505  -7.8995  d=   0.0831
 18:   1.9372   2.9616  -8.0339  d=   0.0926
 19:   3.0232  -5.9846   3.0097  d=   0.1157
 20:   3.1014   0.0442   5.8588  d=   0.0953
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 17718 observations read
Component 2: 17579 observations read

27652 composite observations collected (20130 fully isolated, 7522 overlapped), 52 skipped due to one or more missing parts and 38 skipped due to I/sig<-3.0

OVERLAP STATISTICS

2 COMPONENTS

COMPONENTS 1, 2
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |       3634 |    13.1 <--- ALMOST SEPARATED
   0.20 - 0.40  |       2237 |     8.1
   0.40 - 0.60  |        954 |     3.5
   0.60 - 0.80  |        482 |     1.7
   0.80 - 1.00  |        215 |     0.8 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |       7522 |    27.2

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 94.00% (8434 common observations, 2645 merged)
Twin 2: 6.00% (5455 common observations, 2645 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

16016 of 17659 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-136859.1563 max=39508968.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=75.7644 max=171132.6719

SCALING COMPONENT 2

16026 of 17515 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-8794556.0000 max=39508968.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=73.2553 max=171132.6719
PROFFIT INFO: 359 observations on 'bad frames' rejected

Computed twin ratios:
Twin 1: 95.48% (8418 common observations, 2639 merged)
Twin 2: 4.52% (5362 common observations, 2639 merged)

DC PROFFITRRPTWIN INFO: Determining HKLF4 overlap threshold for completeness requirement (>=80.0%)
DC PROFFITRRPTWIN INFO: HKLF4 overlap threshold kept - 0.40

DC PROFFITRRPTWIN INFO: Step 6 - Decomposed intensities statistics (HKLF4)
 
COMPONENT 1

 
Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only!
	Mean F2 and F2/sig(F2) are given for all measured values!
Note: The RsigmaA values are computed for all measured values!

Help: For more information about computations of rint and rsigma please look into Crysalis help: 
 file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html
 

Statistics vs intensity - point group symmetry: P-1
                       #        #        #      average    mean      mean        
          intensity measured   kept    unique  redundancy   F2     F2/sig(F2)   Rint   Rsigma
---------------------------------------------------------------------------------------------
  39508968-  2581075     1589     1589      564    2.8   5608723.79   125.60    0.032    0.033
   2580578-  1430148     1690     1690      564    3.0   1913083.64    69.43    0.034    0.037
   1429876-   913214     1644     1644      564    2.9   1162644.28    53.75    0.035    0.038
    913059-   593390     1631     1631      564    2.9    742443.62    43.88    0.037    0.041
    593010-   373569     1585     1585      564    2.8    475160.10    34.14    0.045    0.047
    373461-   214020     1601     1601      564    2.8    288065.27    25.86    0.048    0.052
    213858-   113127     1595     1595      564    2.8    161971.72    18.37    0.059    0.061
    113123-    50501     1624     1624      564    2.9     79510.42    11.31    0.083    0.088
     50495-    16522     1540     1540      564    2.7     31576.24     5.71    0.153    0.161
     16490-    -5562     1517     1517      566    2.7      7209.39     1.51    0.396    0.419
-------------------------------------------------------------------------------------------
  39508968-    -5562    16016    16016     5642    2.8   1057008.07    39.41    0.036    0.038
 

Statistics vs resolution - point group symmetry: P-1
resolu-      #        #        #               average    mean      mean          
tion(A)   measured   kept    unique           redundancy   F2     F2/sig(F2)   Rint   Rsigma   RsigmaA
------------------------------------------------------------------------------------------------------
 inf-1.69     1457     1457      564             2.6   3243582.71    98.93    0.036    0.038     0.007
1.69-1.36     1170     1170      564             2.1   1774882.38    50.17    0.029    0.029     0.013
1.36-1.20     2171     2171      564             3.8   1382342.09    41.69    0.040    0.046     0.017
1.20-1.09     2005     2005      564             3.6    926786.65    32.88    0.036    0.040     0.020
1.09-1.02     1767     1767      564             3.1    699479.68    28.63    0.030    0.033     0.024
1.02-0.96     1754     1754      564             3.1    737880.05    30.68    0.028    0.031     0.022
0.96-0.91     1628     1628      564             2.9    654742.16    30.34    0.035    0.037     0.022
0.91-0.87     1508     1508      564             2.7    476332.34    28.27    0.036    0.038     0.025
0.87-0.84     1386     1386      564             2.5    398505.33    28.64    0.051    0.052     0.025
0.84-0.81     1170     1170      566             2.1    342288.06    30.53    0.046    0.048     0.023
------------------------------------------------------------------------------------------------------
 inf-0.81    16016    16016     5642             2.8   1057008.07    39.41    0.036    0.038     0.016
 

Statistics vs resolution (taking redundancy into account) - point group symmetry: P-1
resolu-      #        #        #       %       average    mean      mean          
tion(A)    kept     theory   unique complete  redundancy   F2     F2/sig(F2)   Rint  RsigmaB
--------------------------------------------------------------------------------------------
 inf-1.69     1457      646      564   87.3      2.6   3243582.71   157.95    0.036    0.005
1.69-1.36     1170      598      564   94.3      2.1   1774882.38    72.61    0.029    0.009
1.36-1.20     2171      585      564   96.4      3.8   1382342.09    84.02    0.040    0.009
1.20-1.09     2005      579      564   97.4      3.6    926786.65    63.66    0.036    0.011
1.09-1.02     1767      580      564   97.2      3.1    699479.68    51.67    0.030    0.013
1.02-0.96     1754      577      564   97.7      3.1    737880.05    55.24    0.028    0.013
0.96-0.91     1628      581      564   97.1      2.9    654742.16    53.01    0.035    0.013
0.91-0.87     1508      578      564   97.6      2.7    476332.34    47.76    0.036    0.015
0.87-0.84     1386      579      564   97.4      2.5    398505.33    46.22    0.051    0.016
0.84-0.81     1170      599      566   94.5      2.1    342288.06    46.55    0.046    0.015
--------------------------------------------------------------------------------------------
 inf-0.81    16016     5903     5642   95.6      2.8   1057008.07    68.07    0.036    0.010
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=17657, from those 16015 with overlapping factor < 0.400 written to file D:\Data\xs0936a\xs0936a_max_abs_twin1_hklf4.hkl, 1642 skipped
Use the HKLF 4 file(s) for structure solution.

HKLF 5 merged
RINT ANALYSIS FOR ALL HKLF5 REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2          17658     16068      8723     1.84     38.49     0.021     0.017

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2           7302      6573      4023     1.63     42.35     0.022     0.015

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
     1       10356      9495      4700     2.02     35.50     0.020     0.018
     2           0         0         0     0.00      0.00     0.000     0.000

8723 merged reflections saved into file: D:\Data\xs0936a\xs0936a_max_abs_twin1_hklf5.hkl

Use this hkl file in SHELXL with BASF instruction, which has (components minus 1) entries, and HKLF 5 instruction.
E.g. Two component twin: 'BASF n2' in .ins file, BASF n1 can be computed as n1 = 1.0 - n2.
E.g. Three component twin: 'BASF n2 n3' in .ins file, BASF n1 can be computed as n1 = 1.0 - (n2 + n3).

BASF 0.04522 
;
_shelx_res_checksum              46241
_shelx_hkl_checksum              7753