Synthesis and crystal structure of bis(μ2-acetato-κ2 O:O′)–bis(μ2–(8-(2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)naphthalen-2-olato-κ6 O:O,N,N′,O′:O′)tricobalt(II), C44H38Co3N4O12
Ren, Zong-Li; Mu, Hao-Ran; An, Xiao-Xin; Peng, Yun-Dong; Dong, Wen-Kui; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 15–17; doi:10.1515/ncrs-2017-0394

data_8105525
_publ_section_title
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 Synthesis and crystal structure of bis(\m2-acetato-\k2
 O:O&#x2032;)--bis(\m2--(8-(2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)naphthalen-2-olato-\k6
 O:O,N,N&#x2032;,O&#x2032;:O&#x2032;)tricobalt(II), C44H38Co3N4O12
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              15
_journal_page_last               17
_journal_paper_doi               10.1515/ncrs-2017-0394
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C44 H38 Co3 N4 O12'
_chemical_formula_sum            'C44 H38 Co3 N4 O12'
_chemical_formula_weight         991.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.916(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1982(8)
_cell_length_b                   14.1334(7)
_cell_length_c                   18.7433(11)
_cell_measurement_reflns_used    1466
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      24.4710
_cell_measurement_theta_min      3.8340
_cell_volume                     4082.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -89.00  -58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  178.0000 -150.0000 31

  2 omega   42.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000 -150.0000 53

  3 omega   14.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   57.0000 -150.0000 59

  4 omega    8.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   57.0000  -60.0000 84

  5 omega   48.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000  120.0000 36
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0199200000
_diffrn_orient_matrix_UB_12      0.0447643000
_diffrn_orient_matrix_UB_13      -0.0004390000
_diffrn_orient_matrix_UB_21      0.0143707000
_diffrn_orient_matrix_UB_22      0.0007109000
_diffrn_orient_matrix_UB_23      0.0397513000
_diffrn_orient_matrix_UB_31      0.0389388000
_diffrn_orient_matrix_UB_32      0.0226978000
_diffrn_orient_matrix_UB_33      -0.0004101000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8736
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+6.7546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                2647
_reflns_number_total             4011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0394_suppl.cif
_cod_data_source_block           w75
_cod_database_code               8105525
_reflns_odcompleteness_completeness 99.73
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_olex2_date_sample_data_collection 2017-09-28
_olex2_submission_special_instructions 'No special instructions were received'