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_4349470
_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            'C44 H41 B2 Cu F8 N7'
_chemical_formula_weight         905.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5185(8)
_cell_length_b                   18.7898(14)
_cell_length_c                   19.2943(14)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.16
_cell_volume                     4175.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31700
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.988
_diffrn_reflns_theta_min         2.059
_diffrn_source                   '30 W microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.31
_refine_diff_density_rms         0.05
_refine_ls_abs_structure_details
;
 Flack x determined using 3033 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.033
_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^)+(0.0473P)^2^+1.0352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.086
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                7389
_reflns_number_total             8009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00079g2.cif
_cod_data_source_block           lp644b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4349470
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-4