Crystal Structure of a Dinuclear Co Complex with Doubly Bridged Fluorides: Di-μ-fluoride Bis{(2-pyridylmethyl)bis(2-quinolylmethyl)amine} Dicobalt(II) Bis(tetrafluoroborate), [Co<sub>2</sub>(μ-F)<sub>2</sub>(pbqa)<sub>2</sub>](BF<sub>4</sub>)<sub>2</sub>
MIBU, Takuto; SUENAGA, Yusaku; OKUBO, Takashi; MAEKAWA, Masahiko; KURODA-SOWA, Takayoshi; X-ray Structure Analysis Online 35 (2019) 61–; doi:10.2116/xraystruct.35.61

data_1552778
_publ_section_title
;
 Crystal Structure of a Dinuclear Co Complex with Doubly Bridged
 Fluorides: Di-\m-fluoride
 Bis{(2-pyridylmethyl)bis(2-quinolylmethyl)amine} Dicobalt(II)
 Bis(tetrafluoroborate),
 [Co&lt;sub&gt;2&lt;/sub&gt;(\m-F)&lt;sub&gt;2&lt;/sub&gt;(pbqa)&lt;sub&gt;2&lt;/sub&gt;](BF&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              61
_journal_paper_doi               10.2116/xraystruct.35.61
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety
'C4 H10 O, C H4 O, C52 H44 Co2 F2 N8, 2(B F4)'
_chemical_formula_sum            'C57 H58 B2 Co2 F10 N8 O2'
_chemical_formula_weight         1216.59
_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
_audit_creation_date             2019-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.439(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.9600(9)
_cell_length_b                   11.1533(3)
_cell_length_c                   20.0575(6)
_cell_measurement_reflns_used    11380
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      31.5100
_cell_measurement_theta_min      2.7330
_cell_volume                     5265.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -26.00  46.00   0.50   15.37    --    0.10  77.00-180.00  144
  2  \w     20.00  58.00   0.50   15.37    --    0.10  38.00  30.00   76
  3  \w     45.00  87.00   0.50   15.37    --    0.10  38.00 -90.00   84
  4  \w    -17.00  24.00   0.50   15.37    --    0.10  57.00 -60.00   82
  5  \w    -15.00  45.00   0.50   15.37    --    0.10  57.00  60.00  120
  6  \w     21.00  46.00   0.50   15.37    --    0.10  77.00-150.00   50
  7  \w     -1.00  26.00   0.50   15.37    --    0.10  77.00 -60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0030025000
_diffrn_orient_matrix_UB_12      -0.0630963000
_diffrn_orient_matrix_UB_13      0.0047725000
_diffrn_orient_matrix_UB_21      0.0128023000
_diffrn_orient_matrix_UB_22      0.0083762000
_diffrn_orient_matrix_UB_23      0.0370310000
_diffrn_orient_matrix_UB_31      -0.0271130000
_diffrn_orient_matrix_UB_32      -0.0029466000
_diffrn_orient_matrix_UB_33      0.0040384000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38468
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         31.345
_diffrn_reflns_theta_min         3.062
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7897
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+9.8364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7176
_reflns_number_total             7897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_61_1.txt
_cod_data_source_block           m4-8-co2myu-fpbqabf430c-2
_cod_database_code               1552778
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N B F Co O'
_exptl_absorpt_special_details   block
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All O(H) groups
2. Restrained distances
 B1A-F2A \\sim B1A-F3A \\sim B1A-F4A \\sim B1A-F5A
 with sigma of 0.02
 F2A-F3A \\sim F2A-F4A \\sim F2A-F5A \\sim F3A-F4A \\sim F3A-F5A \\sim F4A-F5A
 with sigma of 0.02
 B1B-F2B \\sim B1B-F3B \\sim B1B-F4B \\sim B1B-F5B
 with sigma of 0.02
 F2B-F3B \\sim F2B-F4B \\sim F2B-F5B \\sim F3B-F4B \\sim F3B-F5B \\sim F4B-F5B
 with sigma of 0.02
3. Others
 Sof(B1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=1-FVAR(1)
 Sof(B1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=FVAR(1)
 Fixed Sof: O1(0.5) C28(0.5) H28A(0.5) H28B(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C29(0.5) H29A(0.5) H29B(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 O2(0.5) H2(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C1(H1A,H1B), C7(H7A,H7B), C17(H17A,H17B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25)
4.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              27079
_shelx_hkl_checksum              79760
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.751
_oxdiff_exptl_absorpt_empirical_full_min 0.587