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_7042927
_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 Br2 Cr2 N4 O6'
_chemical_formula_sum            'C24 H20 Br2 Cr2 N4 O6'
_chemical_formula_weight         724.26
_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   geom
_audit_creation_date             2015-11-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_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                   7.8068(2)
_cell_length_b                   12.2423(4)
_cell_length_c                   13.3916(4)
_cell_measurement_reflns_used    4892
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.5150
_cell_measurement_theta_min      4.2070
_cell_volume                     1279.88(7)
_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 0.919
_diffrn_measurement_details
;
  1 omega  -20.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000    0.0000 51

  2 omega  -62.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000  -90.0000 95

  3 omega  -62.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000  120.0000 93

  4 omega  -58.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -57.0000   30.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0454592000
_diffrn_orient_matrix_UB_12      0.0498867000
_diffrn_orient_matrix_UB_13      -0.0051834000
_diffrn_orient_matrix_UB_21      -0.0137915000
_diffrn_orient_matrix_UB_22      -0.0114767000
_diffrn_orient_matrix_UB_23      -0.0512829000
_diffrn_orient_matrix_UB_31      -0.0774340000
_diffrn_orient_matrix_UB_32      -0.0271752000
_diffrn_orient_matrix_UB_33      0.0121500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11349
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.769
_diffrn_reflns_theta_min         3.042
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83855
_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            'light purple'
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by solvothermal methods'
_exptl_crystal_size_max          0.2406
_exptl_crystal_size_mid          0.0961
_exptl_crystal_size_min          0.0943
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 1252 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0169P)^2^+0.7893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                3011
_reflns_number_total             3209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           3
_cod_database_code               7042927
_chemical_oxdiff_formula         'C30 H30 N4 O10 Cr Br'
_chemical_oxdiff_usercomment     '@ 120 K 240o'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              26034
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_submission    2015-11-23
_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 240o
_olex2_submission_special_instructions 'No special instructions were received'