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_7042925
_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         'C14 H20 Cl4 Cr2 N2 O4, 2(C2 H3 N)'
_chemical_formula_sum            'C18 H26 Cl4 Cr2 N4 O4'
_chemical_formula_weight         608.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-08
_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                112.400(4)
_cell_angle_beta                 101.243(3)
_cell_angle_gamma                102.099(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2906(3)
_cell_length_b                   8.5467(3)
_cell_length_c                   10.1679(4)
_cell_measurement_reflns_used    5690
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      73.2890
_cell_measurement_theta_min      4.9160
_cell_volume                     620.48(5)
_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
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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)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_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 0.985
_diffrn_measurement_details
;
  1 omega  -50.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  120.0000 79

  2 omega  -50.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -90.0000 79

  3 omega -122.00   -6.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -19.0000  -60.0000 116

  4 omega   12.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686   77.0000  -30.0000 105

  5 omega   27.00  101.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -130.0000  142.0000 74

  6 omega   23.00   98.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000 -150.0000 75

  7 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 59

  8 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

  9 omega   41.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  150.0000 98

 10 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 59

 11 omega   40.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -130.0000  142.0000 84

 12 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  120.0000 55

 13 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 59

 14 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 91

 15 omega   94.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -120.0000 84

 16 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 55

 17 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 82

 18 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

 19 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000    0.0000 91

 20 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

 21 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  120.0000 91

 22 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  150.0000 91

 23 omega   37.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -30.0000 105

 24 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   60.0000 55

 25 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 82

 26 omega -117.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   60.0000 105

 27 omega -113.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000  120.0000 96

 28 omega -113.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -150.0000 96

 29 omega -117.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  -30.0000 105

 30 omega    1.00   83.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000    0.0000 82

 31 omega   87.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -60.0000 41

 32 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0690679000
_diffrn_orient_matrix_UB_12      -0.0880201000
_diffrn_orient_matrix_UB_13      -0.1718058000
_diffrn_orient_matrix_UB_21      -0.0237423000
_diffrn_orient_matrix_UB_22      0.1758822000
_diffrn_orient_matrix_UB_23      0.0047308000
_diffrn_orient_matrix_UB_31      0.1856334000
_diffrn_orient_matrix_UB_32      0.0588079000
_diffrn_orient_matrix_UB_33      -0.0071201000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.392
_diffrn_reflns_theta_min         4.938
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69348
_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    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             310
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and hexane by vapour diffusion'
_exptl_crystal_size_max          0.0925
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.0399
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0050(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0837P)^2^+0.3629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2421
_reflns_number_total             2577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           7
_cod_original_cell_volume        620.49(4)
_cod_database_code               7042925
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cr Cl B Na'
_chemical_oxdiff_usercomment     '@ 120 K 152'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.84 with sigma of 0.02
 H2A-H2B
 1.35 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              34848
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_submission    2015-10-07
_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 152
_olex2_submission_special_instructions 'No special instructions were received'