Magneto-structural correlations in a family of dialkoxo bridged chromium dimers
Brechin, Euan K.; Fraser, Hector; Nichol, Gary Stephen; Velmurugan, Gunasekaran; Rajaraman, Gopalan; Dalton Trans.  (2017) –; doi:10.1039/C7DT01197K

data_7042923
_publ_section_title
;
 Magneto-structural correlations in a family of dialkoxo bridged chromium
 dimers
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01197K
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C11 H11 Cl2 Cr N2 O), 2(C5 H5 N)'
_chemical_formula_sum            'C32 H32 Cl4 Cr2 N6 O2'
_chemical_formula_weight         778.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2418(2)
_cell_length_b                   16.2418(2)
_cell_length_c                   25.6069(6)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.7900
_cell_measurement_theta_min      5.1490
_cell_volume                     6755.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -122.00  -6.00   1.00    5.00    --  -43.17 -19.00 150.00  116
  2  \w   -113.00 -17.00   1.00    5.00    --  -43.17 -57.00 -60.00   96
  3  \w    -70.00  27.00   1.00    5.00    --  -43.17  57.00  90.00   97
  4  \w     87.00 178.00   1.00   20.00    --  111.00  45.00-120.00   91
  5  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00-120.00  105
  6  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00   0.00  105
  7  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00-150.00   79
  8  \w     36.00 135.00   1.00   20.00    --  111.00 -30.00  30.00   99
  9  \w     87.00 178.00   1.00   20.00    --  111.00  45.00   0.00   91
 10  \w     40.00 135.00   1.00   20.00    --  111.00 -45.00 -90.00   95
 11  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00 120.00  105
 12  \w     94.00 178.00   1.00   20.00    --  111.00 125.00 -60.00   84
 13  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00 -30.00   79
 14  \w    106.00 160.00   1.00   20.00    --  111.00 125.00-180.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0493161000
_diffrn_orient_matrix_UB_12      0.0465783000
_diffrn_orient_matrix_UB_13      0.0420147000
_diffrn_orient_matrix_UB_21      -0.0015276000
_diffrn_orient_matrix_UB_22      0.0769691000
_diffrn_orient_matrix_UB_23      -0.0351145000
_diffrn_orient_matrix_UB_31      -0.0810507000
_diffrn_orient_matrix_UB_32      -0.0298702000
_diffrn_orient_matrix_UB_33      -0.0249563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28737
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.316
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.539
_exptl_absorpt_correction_T_max  0.7789
_exptl_absorpt_correction_T_min  0.3885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1121 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.4988.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of pyridine and diethyl ether by vapour diffusion'
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+21.3008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5590
_reflns_number_total             6396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           5
_cod_database_code               7042923
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K 589'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.41(3) 0.097(19) 0.089(19) 0.400(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid body (RIGU) restrains
 N5, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C28, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, N3, C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, N1, C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl3A)=Sof(Cl4A)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32)
5.c Fitted hexagon refined as free rotating group:
 N5(C23,C24,C25,C26,C27), N6(C28,C29,C30,C31,C32)
;
_shelx_res_checksum              25364
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-29
_olex2_date_sample_submission    2016-04-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id 589
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.651