On the fly multi-modal observation of ligand synthesis and complexation of Cu complexes in flow with ‘benchtop’ NMR and mass spectrometry
Porwol, Luzian; Henson, Alon; Kitson, Philip J.; Long, De-Liang; Cronin, Leroy; Inorganic Chemistry Frontiers 3 (2016) 919–; doi:10.1039/C6QI00079G

data_4349472
_publ_section_title
;
 On the fly multi-modal observation of ligand synthesis and complexation
 of Cu complexes in flow with &#x2018;benchtop&#x2019; NMR and mass
 spectrometry
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              919
_journal_paper_doi               10.1039/C6QI00079G
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C53 H48 B2 Cu2 F8 N8 O3'
_chemical_formula_weight         1145.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   'F map'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-02-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.726(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_c                   16.4909(12)
_cell_measurement_reflns_used    2532
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.36
_cell_volume                     2512.6(3)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    dimond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
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_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31718
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         2.014
_diffrn_source                   '30 W microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.111
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+12.9193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.155
_refine_ls_wR_factor_ref         0.166
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00079g2.cif
_cod_data_source_block           lp118
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349472
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.964
_shelxl_version_number           2013-4