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_7042922
_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         'C24 H20 Cl2 Cr2 N4 O6'
_chemical_formula_sum            'C24 H20 Cl2 Cr2 N4 O6'
_chemical_formula_weight         635.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-10-20
_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            2
_cell_length_a                   7.81306(10)
_cell_length_b                   12.17220(15)
_cell_length_c                   13.10384(16)
_cell_measurement_reflns_used    25916
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      32.7020
_cell_measurement_theta_min      4.2170
_cell_volume                     1246.20(3)
_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      120.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -48.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248   24.0000 -166.7022 107

  2 omega  -12.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   77.0000   60.0000 105

  3 omega  -12.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   77.0000   30.0000 105

  4 omega  -20.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -99.0000    0.0000 79

  5 omega    3.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311 -126.0000 -176.6475 72

  6 omega   -4.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   38.0000  -30.0000 96

  7 omega   17.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311 -154.0000  -85.2487 77

  8 omega  -78.00  -29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  133.0000 -102.0130 49

  9 omega  -91.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  -77.0000  150.0000 105

 10 omega  -54.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -38.0000  -90.0000 95

 11 omega  -54.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -38.0000   30.0000 95

 12 omega  -20.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -99.0000   60.0000 79

 13 omega   -8.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311 -113.0000   34.2842 39

 14 omega   -8.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   57.0000 -150.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0038168000
_diffrn_orient_matrix_UB_12      0.0432639000
_diffrn_orient_matrix_UB_13      0.0361701000
_diffrn_orient_matrix_UB_21      -0.0315923000
_diffrn_orient_matrix_UB_22      -0.0371701000
_diffrn_orient_matrix_UB_23      0.0372022000
_diffrn_orient_matrix_UB_31      0.0850270000
_diffrn_orient_matrix_UB_32      -0.0118985000
_diffrn_orient_matrix_UB_33      0.0154309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45650
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.892
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93711
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.3263
_exptl_crystal_size_mid          0.1812
_exptl_crystal_size_min          0.1783
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 2032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0275P)^2^+0.2734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                4406
_reflns_number_total             4514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           2
_cod_database_code               7042922
_chemical_oxdiff_formula         'C30 H30 N2 O5 Cr2 Cl2 '
_chemical_oxdiff_usercomment     '@ 120 K 1960 (or 1950 as written on vial) '
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              81863
_shelx_shelxl_version_number     2014/7
_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 '1960 (1950 on vial)'
_olex2_submission_special_instructions 'No special instructions were received'