Syntheses, structures and magnetic properties of four manganese(ii) and cobalt(ii) complexes
Hu, Tuoping; Zheng, Baohua; Wang, Xiaoqing; Hao, Xuena; CrystEngComm 17 (2015) 9348–; doi:10.1039/C5CE01857A

data_7223098
_publ_section_title
;
 Syntheses, structures and magnetic properties of four manganese(ii) and
 cobalt(ii) complexes
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              9348
_journal_paper_doi               10.1039/C5CE01857A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C23 H18 Mn N2 O6, H2 O'
_chemical_formula_sum            'C23 H20 Mn N2 O7'
_chemical_formula_weight         491.35
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-01-25 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                96.781(7)
_cell_angle_beta                 94.868(7)
_cell_angle_gamma                110.509(7)
_cell_formula_units_Z            2
_cell_length_a                   7.7565(6)
_cell_length_b                   9.5643(8)
_cell_length_c                   15.1895(14)
_cell_measurement_reflns_used    1852
_cell_measurement_temperature    298.5(4)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.93
_cell_volume                     1038.34(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      298.5(4)
_diffrn_detector_area_resol_mean 16.0450
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   16.00   48.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  -86.0000  -34.0556 32

  2 omega  -48.00   21.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  -57.0000 -150.0000 69

  3 omega  -30.00   85.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251   19.0000   30.0000 115

  4 omega   50.00   97.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  178.0000 -120.0000 47

  5 omega   -2.00   84.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251   57.0000   90.0000 86

  6 omega   -2.00   24.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251   57.0000  -30.0000 26

  7 omega  -20.00   24.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9813  -99.0000 -180.0000 44

  8 omega  -77.00  -51.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9813  -19.0000   60.0000 26

  9 omega  -55.00  -30.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  -19.0000  -60.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0359309000
_diffrn_orient_matrix_UB_12      0.0521064000
_diffrn_orient_matrix_UB_13      0.0403422000
_diffrn_orient_matrix_UB_21      0.0482202000
_diffrn_orient_matrix_UB_22      0.0567779000
_diffrn_orient_matrix_UB_23      -0.0245570000
_diffrn_orient_matrix_UB_31      -0.0780717000
_diffrn_orient_matrix_UB_32      0.0221803000
_diffrn_orient_matrix_UB_33      -0.0047318000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8071
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            faint-yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                2495
_reflns_number_total             3631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01857a2.cif
_cod_data_source_block           htp-f14
_cod_depositor_comments
'Adding full bibliography for 7223097--7223100.cif.'
_cod_original_cell_volume        1038.33(15)
_cod_database_code               7223098
_audit_block_doi                 10.5517/cc141rtr
_chemical_oxdiff_formula         'C H O N Co'
_reflns_odcompleteness_completeness 99.79
_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 O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O3W(H3WA,H3WB)
2.b Rotating group:
 O2W(H2WB), O1W(H1WB,H1WA)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C17(H17), C18(H18), C10(H10), C20(H20), C4(H4), C0AA(H0AA), C13(H13),
 C5(H5), C2(H2), C11(H11), C14(H14), C8(H8), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'