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_7042924
_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         'C12 H13 Cl2 Cr N2 O2'
_chemical_formula_sum            'C14 H16 Cl2 Cr N3 O2'
_chemical_formula_weight         381.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           133
_space_group_name_Hall           '-P 4ac 2b'
_space_group_name_H-M_alt        'P 42/n b c'
_symmetry_space_group_name_Hall  '-P 4ac 2b'
_symmetry_space_group_name_H-M   'P 42/n b c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_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                   15.4761(3)
_cell_length_b                   15.4761(3)
_cell_length_c                   12.3453(3)
_cell_measurement_reflns_used    24294
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.1690
_cell_measurement_theta_min      3.7150
_cell_volume                     2956.82(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -92.00  -51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  173.0000  -53.1619 41

  2 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  150.0000 51

  3 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000   60.0000 51

  4 omega  -73.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  140.0000 -123.8148 41

  5 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  120.0000 51

  6 omega  -68.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -19.0000   60.0000 116

  7 omega  -59.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -57.0000    0.0000 96

  8 omega  -12.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   38.0000 -180.0000 95

  9 omega   13.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -145.0000 -131.5234 65

 10 omega  -62.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000 -180.0000 95

 11 omega  -66.00  -25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  127.0000   39.2654 41

 12 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000 -150.0000 51

 13 omega  -83.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -77.0000    0.0000 105

 14 omega   -5.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -117.0000   62.3225 66

 15 omega  -16.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   57.0000  -60.0000 97

 16 omega    4.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -128.0000  -32.3956 64

 17 omega    6.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -131.0000 -111.6368 64

 18 omega  -20.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -99.0000  -90.0000 71

 19 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000   30.0000 51

 20 omega  -62.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000 -150.0000 95

 21 omega    9.00   73.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -137.0000  112.1175 64

 22 omega    3.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -127.0000  -67.2231 64

 23 omega    6.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -131.0000 -179.0000 64

 24 omega   10.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -138.0000    4.0000 47

 25 omega    6.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -130.0000   14.0926 63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0258217000
_diffrn_orient_matrix_UB_12      -0.0374303000
_diffrn_orient_matrix_UB_13      0.0072672000
_diffrn_orient_matrix_UB_21      -0.0369078000
_diffrn_orient_matrix_UB_22      -0.0264181000
_diffrn_orient_matrix_UB_23      -0.0079844000
_diffrn_orient_matrix_UB_31      0.0085227000
_diffrn_orient_matrix_UB_32      -0.0010413000
_diffrn_orient_matrix_UB_33      -0.0564241000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            134457
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and diethyl ether by vapour diffusion'
_exptl_crystal_size_max          0.2229
_exptl_crystal_size_mid          0.0507
_exptl_crystal_size_min          0.0432
_platon_squeeze_details          'MeCN removed'
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.330
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0319P)^2^+7.2479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1516
_reflns_number_total             1520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           8
_cod_original_cell_volume        2956.82(13)
_cod_database_code               7042924
_chemical_oxdiff_formula         'C12 H12 Cl2 Cr N2 O2 '
_chemical_oxdiff_usercomment     '@ 120 K 156'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_platon_squeeze_void_probe_radius 1.20
_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 O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 C6-H1
 1.888082 with sigma of 0.02
 Cr1-H1
 2.650777 with sigma of 0.02
3. Others
 Fixed Sof: H1(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              52489
_shelx_fab_checksum              3078
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-03
_olex2_date_sample_submission    2015-10-09
_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 156
_olex2_submission_special_instructions 'No special instructions were received'