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_7223097
_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         'C41 H34 Co2 N2 O10.25, H2 O'
_chemical_formula_sum            'C41 H36 Co2 N2 O12'
_chemical_formula_weight         866.58
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-04-19 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.509(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.394(3)
_cell_length_b                   13.578(3)
_cell_length_c                   18.261(3)
_cell_measurement_reflns_used    1365
_cell_measurement_temperature    273(2)
_cell_measurement_theta_min      2.75
_cell_volume                     3668.6(12)
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1275
_diffrn_reflns_av_unetI/netI     0.1886
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18223
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1473
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          1.179
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                2819
_reflns_number_total             6438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01857a2.cif
_cod_data_source_block           p
_cod_depositor_comments
'Adding full bibliography for 7223097--7223100.cif.'
_cod_original_cell_volume        3668.5(12)
_cod_database_code               7223097
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1A \\sim O2A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
3. Others
 Fixed Sof: O1A(0.5) O2A(0.75)
4.a Free rotating group:
 O13(H13A,H13B)
4.b Rotating group:
 O9(H9A,H9B), O11(H11A,H11B), O12(H12A,H12B)
4.c Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C55(H55A,H55B), C59(H59A,H59B)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C13(H13), C14(H14), C20(H20), C22(H22), C25(H25), C28(H28), C29(H29),
 C30(H30), C32(H32), C36(H36), C38(H38), C43(H43), C47(H47), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C57(H57), C60(H60), C66(H66)
;