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_7042929
_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_formula_moiety         '2(C12 H13 Cl2 Cr N2 O)'
_chemical_formula_sum            'C24 H26 Cl4 Cr2 N4 O2'
_chemical_formula_weight         648.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.3958(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.29325(19)
_cell_length_b                   14.06348(14)
_cell_length_c                   14.8511(2)
_cell_measurement_reflns_used    23006
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.9260
_cell_measurement_theta_min      3.3310
_cell_volume                     2650.46(7)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.986
_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    -96.00  -2.00   1.00    5.00    --  -43.17 125.00 -90.00   94
  2  \w   -113.00 -17.00   1.00    5.00    --  -43.17 -57.00-150.00   96
  3  \w   -116.00 -21.00   1.00    5.00    --  -43.17 -38.00  90.00   95
  4  \w     17.00 113.00   1.00    5.00    --   43.17  57.00  30.00   96
  5  \w     40.00 135.00   1.00   20.00    --  111.00 -45.00-120.00   95
  6  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00-150.00   79
  7  \w     87.00 178.00   1.00   20.00    --  111.00  30.00-180.00   91
  8  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00  30.00  105
  9  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00-120.00   79
 10  \w     87.00 178.00   1.00   20.00    --  111.00  30.00 -90.00   91
 11  \w   -113.00 -17.00   1.00    5.00    --  -43.17 -57.00 -60.00   96
 12  \w    -66.00  29.00   1.00    5.00    --  -43.17  38.00 -90.00   95
 13  \w    -66.00  29.00   1.00    5.00    --  -43.17  38.00-180.00   95
 14  \w     87.00 178.00   1.00   20.00    --  111.00  30.00 120.00   91
 15  \w     80.00 178.00   1.00   20.00    --  111.00  77.00 -60.00   98
 16  \w     83.00 178.00   1.00   20.00    --  111.00  61.00-150.00   95
 17  \w     39.00 121.00   1.00   20.00    --  111.00-125.00  60.00   82
 18  \w     83.00 178.00   1.00   20.00    --  111.00  61.00  60.00   95
 19  \w     66.00 178.00   1.00   20.00    --  111.00  15.00  60.00  112
 20  \w   -117.00 -12.00   1.00    5.00    --  -43.17 -77.00 150.00  105
 21  \w    -66.00  29.00   1.00    5.00    --  -43.17  38.00  90.00   95
 22  \w   -117.00 -12.00   1.00    5.00    --  -43.17 -77.00  60.00  105
 23  \w     83.00 178.00   1.00   20.00    --  111.00  61.00 120.00   95
 24  \w     80.00 178.00   1.00   20.00    --  111.00  77.00   0.00   98
 25  \w     83.00 178.00   1.00   20.00    --  111.00  61.00-180.00   95
 26  \w     30.00 102.00   1.00   20.00    --  111.00 -94.00 120.00   72
 27  \w     83.00 178.00   1.00   20.00    --  111.00  61.00 -30.00   95
 28  \w     83.00 178.00   1.00   20.00    --  111.00  61.00 -90.00   95
;
_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      -0.1202101000
_diffrn_orient_matrix_UB_12      -0.0093843000
_diffrn_orient_matrix_UB_13      -0.0648485000
_diffrn_orient_matrix_UB_21      0.0029401000
_diffrn_orient_matrix_UB_22      0.0743698000
_diffrn_orient_matrix_UB_23      -0.0748320000
_diffrn_orient_matrix_UB_31      0.0169558000
_diffrn_orient_matrix_UB_32      -0.0798628000
_diffrn_orient_matrix_UB_33      -0.0619545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43244
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.778
_diffrn_reflns_theta_min         3.142
_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    10.720
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_correction_T_min  0.5795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0953 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.5958.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of 4-picoline and diethyl ether by vapour diffusion'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0806P)^2^+1.2782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5054
_reflns_number_total             5513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           6
_cod_database_code               7042929
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     '@ 120 K 679'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C56(H56A,H56B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C51(H51),
 C52(H52), C53(H53), C54(H54), C57(H57), C58(H58), C60(H60), C61(H61)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C62(H62A,H62B,H62C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-05
_olex2_date_sample_submission    2016-08-05
_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 679
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.655
_oxdiff_exptl_absorpt_empirical_full_min 0.770