Crystal structure of bis(μ2-acetato-κ2 O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6 O:O,N,N′,O′′:O′′}tricobalt(II), C44H49Cl2Co3N6O12
Yang, Yu-Hua; Wang, Bao-Jun; Lan, Peng-Fei; Dong, Wen-Kui; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 869–872; doi:10.1515/ncrs-2017-0034

data_8106705
_publ_section_title
;
 Crystal structure of bis(\m2-acetato-\k2
 O:O&#x2032;)-bis{\m2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-\k6
 O:O,N,N&#x2032;,O&#x2032;&#x2032;:O&#x2032;&#x2032;}tricobalt(II),
 C44H49Cl2Co3N6O12
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              869
_journal_page_last               872
_journal_paper_doi               10.1515/ncrs-2017-0034
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C44 H49 Cl2 Co3 N6 O12'
_chemical_formula_sum            'C44 H49 Cl2 Co3 N6 O12'
_chemical_formula_weight         1101.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                72.807(10)
_cell_angle_beta                 83.019(9)
_cell_angle_gamma                72.246(9)
_cell_formula_units_Z            2
_cell_length_a                   9.7415(9)
_cell_length_b                   13.6440(14)
_cell_length_c                   20.277(3)
_cell_measurement_reflns_used    1841
_cell_measurement_temperature    290.92(10)
_cell_measurement_theta_max      21.5690
_cell_measurement_theta_min      3.6980
_cell_volume                     2450.6(5)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      290.92(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -16.00   26.00   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000    0.0000 28

  2 omega  -15.00   25.50   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000 -180.0000 27

  3 omega   44.00   96.50   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946 -178.0000 -150.0000 35

  4 omega  -14.00   20.50   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   19.0000  150.0000 23

  5 omega   36.00   90.00   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  178.0000 -120.0000 36

  6 omega  -46.00   38.00   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -38.0000 -120.0000 56

  7 omega   -4.00   75.50   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   38.0000   30.0000 53

  8 omega  -47.00  -11.00   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -19.0000 -180.0000 24
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0085873000
_diffrn_orient_matrix_UB_12      0.0076564000
_diffrn_orient_matrix_UB_13      -0.0355769000
_diffrn_orient_matrix_UB_21      -0.0386792000
_diffrn_orient_matrix_UB_22      -0.0387675000
_diffrn_orient_matrix_UB_23      0.0086979000
_diffrn_orient_matrix_UB_31      -0.0654389000
_diffrn_orient_matrix_UB_32      0.0407302000
_diffrn_orient_matrix_UB_33      0.0010058000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.1619
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19011
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93546
_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            'clear light brown'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         9620
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                4395
_reflns_number_total             9620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0034_suppl.cif
_cod_data_source_block           d534
_cod_database_code               8106705
_reflns_odcompleteness_completeness 99.71
_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. Uiso/Uaniso restraints and constraints
Uanis(C35') \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36') \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(N6') \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C38') \\sim Ueq, Uanis(C37')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: N6(0.5) C35(0.5) H35a(0.5) H35b(0.5) C36(0.5) H36a(0.5) H36b(0.5)
 H36c(0.5) C37(0.5) H37a(0.5) H37b(0.5) C38(0.5) H38a(0.5) H38b(0.5) H38c(0.5)
 N6'(0.5) C35'(0.5) H35c(0.5) H35d(0.5) C36'(0.5) H36d(0.5) H36e(0.5) H36f(0.5)
 C37'(0.5) H37c(0.5) H37d(0.5) C38'(0.5) H38d(0.5) H38e(0.5) H38f(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C19(H19a,H19b), C28(H28a,H28b), C29(H29a,H29b),
 C35(H35a,H35b), C37(H37a,H37b), C35'(H35c,H35d), C37'(H37c,H37d)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13), C15(H15),
 C17(H17), C22(H22), C23(H23), C25(H25), C27(H27), C30(H30), C32(H32), C33(H33),
  C52(H52)
4.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C20(H20a,H20b,H20c), C40(H40a,H40b,H40c), C42(H42a,H42b,
 H42c), C36(H36a,H36b,H36c), C38(H38a,H38b,H38c), C36'(H36d,H36e,H36f),
 C38'(H38d,H38e,H38f)
;
_olex2_date_sample_data_collection 2014-12-11
_olex2_submission_special_instructions 'No special instructions were received'