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_7042926
_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
'C26 H22 Cr2 N4 O10, 0.5(C H4 O), 0.5 (C4 H10 O)'
_chemical_formula_sum            'C28.5 H29 Cr2 N4 O11'
_chemical_formula_weight         707.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.939(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2931(8)
_cell_length_b                   21.3092(16)
_cell_length_c                   13.2192(8)
_cell_measurement_reflns_used    6609
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      24.3220
_cell_measurement_theta_min      3.3440
_cell_volume                     3312.6(4)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000  120.0000 53

  2 omega  -20.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000   30.0000 53

  3 omega  -20.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000 -180.0000 53

  4 omega  -47.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -57.0000   30.0000 67

  5 omega  -63.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -38.0000  150.0000 57

  6 omega  -42.00  -16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -38.0000  120.0000 26

  7 omega  -24.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   19.0000  120.0000 101

  8 omega   20.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   38.0000  -30.0000 51

  9 omega   47.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   38.0000  150.0000 30

 10 omega  -32.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -38.0000 -150.0000 63

 11 omega    8.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -99.0000 -120.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0041860000
_diffrn_orient_matrix_UB_12      0.0330259000
_diffrn_orient_matrix_UB_13      -0.0067847000
_diffrn_orient_matrix_UB_21      -0.0399259000
_diffrn_orient_matrix_UB_22      0.0011085000
_diffrn_orient_matrix_UB_23      0.0293626000
_diffrn_orient_matrix_UB_31      0.0450073000
_diffrn_orient_matrix_UB_32      0.0040586000
_diffrn_orient_matrix_UB_33      0.0472953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47599
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86992
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_recrystallization_method
'Vapour diffusion from diethyl ether and methanol.'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.0927
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5824
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0830
_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^)+(0.0689P)^2^+17.7889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4892
_reflns_number_total             5824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01197k2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C28.50 H29 Cr2 N4 O11'
_cod_database_code               7042926
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C30 H30 N5 O20 Cr'
_chemical_oxdiff_usercomment     '@ 120 K 860 Ether'
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O11-C27
 1.5 with sigma of 0.02
 O12A-C28 \\sim O12B-C28 \\sim O12B-C30 \\sim O12A-C30
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O11, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12A, O12B, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O11(0.5) H11(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 O12A(0.25) O12B(0.25) C28(0.5) C29(0.5) C30(0.5) C31(0.5)
5.a Riding coordinates:
 O11(H11)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              27390
_olex2_date_sample_data_collection 2015-07-23
_olex2_date_sample_submission    2015-07-20
_olex2_exptl_crystal_mounting_method 'Mitegen tip, Paratone oil.'
_olex2_submission_original_sample_id '860 Ether'
_olex2_submission_special_instructions 'No special instructions were received'