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_7042928
_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(C6 H8 Cl2 Cr N O2), 2(C4 H10 O)'
_chemical_formula_sum            'C20 H36 Cl4 Cr2 N2 O6'
_chemical_formula_weight         646.31
_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             2015-11-06
_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                92.473(4)
_cell_angle_beta                 99.099(4)
_cell_angle_gamma                91.960(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7732(4)
_cell_length_b                   10.4693(3)
_cell_length_c                   14.0067(7)
_cell_measurement_reflns_used    7317
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.1210
_cell_measurement_theta_min      3.4580
_cell_volume                     1412.57(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_details
;
  1 omega  -78.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -57.0000   30.0000 97

  2 omega  -20.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000   30.0000 53

  3 omega  -30.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000 -150.0000 95

  4 omega  -30.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000  120.0000 95

  5 omega  -80.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -38.0000   60.0000 95

  6 omega  -20.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        8.8758  -99.0000  -30.0000 69

  7 omega  -30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000   30.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0650571000
_diffrn_orient_matrix_UB_12      0.0332403000
_diffrn_orient_matrix_UB_13      0.0026154000
_diffrn_orient_matrix_UB_21      -0.0330881000
_diffrn_orient_matrix_UB_22      0.0591741000
_diffrn_orient_matrix_UB_23      0.0011362000
_diffrn_orient_matrix_UB_31      0.0091927000
_diffrn_orient_matrix_UB_32      0.0003376000
_diffrn_orient_matrix_UB_33      0.0512683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6514
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.854
_diffrn_reflns_theta_min         3.288
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of diethyl ether and acetonitrile by vapour diffusion'
_exptl_crystal_size_max          0.1925
_exptl_crystal_size_mid          0.1588
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0728
_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^)+11.0388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5624
_reflns_number_total             6514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           4
_cod_original_cell_volume        1412.58(10)
_cod_database_code               7042928
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K 194'
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.884(2) 0.116(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O52-H52A = O52-H52B = O2-H2B = O2-H2A
 0.84 with sigma of 0.02
 H2A-H2B = H52B-H52A
 1.35 with sigma of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C57(H57A,H57B),
 C59(H59A,H59B)
4.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54), C1(H1), C2(H2), C3(H3), C4(H4)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              90781
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_submission    2015-11-04
_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 194
_olex2_submission_special_instructions 'No special instructions were received'