A series of C3-symmetric heterobimetallic Cr–M (M = Fe, Co and Cu) complexes
Kuppuswamy, Subramaniam; Bezpalko, Mark W.; Powers, Tamara M.; Wilding, Matthew J. T.; Brozek, Carl K.; Foxman, Bruce M.; Thomas, Christine M.; Chemical Science 5 (2014) 1617–; doi:10.1039/c3sc52943f

data_1513868
_publ_section_title
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 A series of C3-symmetric heterobimetallic Cr--M (M = Fe, Co and Cu)
 complexes
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_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1617
_journal_paper_doi               10.1039/c3sc52943f
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C48 H60 Cr1 Fe1 N3 P4'
_chemical_formula_sum            'C48 H60 Cr Fe N3 P4'
_chemical_formula_weight         910.76
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2013-05-29
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   16.2739(3)
_cell_length_b                   16.2739(3)
_cell_length_c                   23.1328(5)
_cell_measurement_reflns_used    6427
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     5305.69(18)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4891
_diffrn_reflns_theta_full        29.409
_diffrn_reflns_theta_max         29.409
_diffrn_reflns_theta_min         1.761
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.210
_platon_squeeze_details
;
During the structure solution, electron density difference maps 
revealed that there were considerable disordered solvent 
molecules which could not be successfully modeled.  From history, 
the remaining solvate was likely ether in a volume of 936.5 \%A3 
per unit cell (17.7%).  It appeared that the cavity area contained 
ca two ether molecules, located near the -3 position at (0, 0, 0). 
Modeling with or without restraints was unsuccessful, as was step 
by step acquisition of peaks using successive electron density 
difference maps.  Thus, the structure factors were modified using 
the PLATON SQUEEZE, technique, in order to produce a "solvate-free" 
structure factor set.  PLATON reported a total electron density 
of 65 e- per unit cell, likely representing two ether molecules, 
consistent with our earlier observations.  Use of the SQUEEZE 
technique resulted in a decrease of ca. 1.5 % in R.   
;
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.0029529
_refine_ls_shift/su_mean         0.0000808
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.21P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0985
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0985
_reflns_limit_h_max              0
_reflns_limit_h_min              -19
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                3444
_reflns_number_total             4891
_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   0.0514
_oxford_refine_ls_scale          0.081450(19)
_oxford_reflns_number_all        4891
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'sk_821rr_0m in P-3c1'
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c3sc52943f.txt
_cod_data_source_block           sk_4
_cod_depositor_comments
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The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
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_cod_original_sg_symbol_Hall     '-P 3 2"c '
_cod_original_sg_symbol_H-M      'P -3 c 1 '
_cod_original_formula_sum        'C48 H60 Cr1 Fe1 N3 P4'
_cod_database_code               1513868