µ-Pyridine bridged Copper Complex with Robust Proton Reducing Ability
Majee, Karunamay; Patel, Jully; Das, Babulal; Padhi, Sumanta Kumar; Dalton Trans.  (2017) –; doi:10.1039/C7DT03153J

data_7044411
_publ_section_title
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 &#x00B5;-Pyridine bridged Copper Complex with Robust Proton Reducing
 Ability
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03153J
_journal_year                    2017
_chemical_formula_moiety         'C50 H30 Cu2 N10 O4, C3 H7 N O, H2 O'
_chemical_formula_sum            'C53 H39 Cu2 N11 O6'
_chemical_formula_weight         1053.05
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-30 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.306(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3335(5)
_cell_length_b                   28.1780(10)
_cell_length_c                   15.8677(6)
_cell_measurement_reflns_used    10079
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.661
_cell_measurement_theta_min      1.445
_cell_volume                     4782.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEX-CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_unetI/netI     0.1504
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.661
_diffrn_reflns_theta_min         1.445
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10079
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0270P)^2^+0.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10058
_reflns_number_total             10079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03153j2.cif
_cod_data_source_block           skp-dmf-11
_cod_database_code               7044411
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 C5, N5, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Free rotating group:
 O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C35(H35), C37(H37), C36(H36), C42(H42), C43(H43), C10(H10),
 C11(H11), C14(H14), C16(H16), C12(H12), C15(H15), C7(H7), C8(H8), C9(H9),
 C48(H48), C47(H47), C46(H46), C27(H27), C28(H28), C29(H29), C21(H21), C22(H22),
  C23(H23), C1(H1), C34(H34), C32(H32), C33(H33), C3(H3), C2(H2), C53(H53)
3.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
;
_olex2_submission_special_instructions 'No special instructions were received'