Microwave−assisted synthesis: from a mononuclear {CoII} complex to {CoII9} solvomorphs
Collet, Alexandra; Wilson, Claire; Murrie, Mark; Dalton Transactions  (2018) –; doi:10.1039/C8DT04557G

data_7048360
_publ_section_title
;
 Microwave&#x2212;assisted synthesis: from a mononuclear {CoII} complex to
 {CoII9} solvomorphs
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04557G
_journal_year                    2018
_chemical_formula_moiety         'C36 H64 Cl4 Co9 N6 O24'
_chemical_formula_sum            'C36 H64 Cl4 Co9 N6 O24'
_chemical_formula_weight         1637.10
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-11-12 deposited with the CCDC.
2018-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.809(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7276(4)
_cell_length_b                   11.8295(3)
_cell_length_c                   15.6451(5)
_cell_measurement_reflns_used    24649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6320
_cell_measurement_theta_min      2.6750
_cell_volume                     2716.10(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -95.00  24.00   1.00    5.00    --   -5.00 -72.00  60.00  119
  2  \w    -29.00  85.00   1.00    5.00    --   -5.00  54.00 150.00  114
  3  \w    -87.00  16.00   1.00    5.00    --   -5.00 -54.00-120.00  103
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0213203000
_diffrn_orient_matrix_UB_12      0.0526514000
_diffrn_orient_matrix_UB_13      -0.0067129000
_diffrn_orient_matrix_UB_21      0.0433036000
_diffrn_orient_matrix_UB_22      -0.0252431000
_diffrn_orient_matrix_UB_23      0.0098431000
_diffrn_orient_matrix_UB_31      0.0022382000
_diffrn_orient_matrix_UB_32      -0.0137631000
_diffrn_orient_matrix_UB_33      -0.0438988000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34254
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.161
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       Block
_exptl_crystal_F_000             1650
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6234
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+3.2120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5718
_reflns_number_total             6234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04557g2.cif
_cod_data_source_block           complex2
_cod_database_code               7048360
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'CoC6 H12 N O4 Cl'
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.798
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.01
 C17-H5
 1.906775 with sigma of 0.02
 Co4-H5
 2.820708 with sigma of 0.02
 C5-H1
 1.910497 with sigma of 0.02
 Co2-H1
 2.811279 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C3(H3A,H3B), C13(H13A,H13B), C2(H2A,H2B),
 C9(H9A,H9B), C8(H8A,H8B), C4(H4A,H4B), C17(H17A,H17B), C6(H6A,H6B), C16(H16A,
 H16B), C18(H18A,H18B), C14(H14A,H14B), C19(H19A,H19B), C5(H5A,H5B)
;
_shelx_res_checksum              16186
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.854
_oxdiff_exptl_absorpt_empirical_full_min 0.677