Structural Characterization and Optical Properties of Two Copper(I)-Iodide BODIPY Coordination Polymers
Hassanain, Hawazen; Davies, Edward Stephen; Lewis, William; Kays, Deborah Lorraine; Champness, Neil R.; CrystEngComm  (2019) –; doi:10.1039/C9CE00845D

data_7232991
_publ_section_title
;
 Structural Characterization and Optical Properties of Two
 Copper(I)-Iodide BODIPY Coordination Polymers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE00845D
_journal_year                    2019
_chemical_formula_moiety         '0.5(C54 H46 B2 Cu4 F4 I4 N12)'
_chemical_formula_sum            'C27 H23 B Cu2 F2 I2 N6'
_chemical_formula_weight         861.20
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-02 deposited with the CCDC.    2019-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.859(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6653(4)
_cell_length_b                   9.0291(3)
_cell_length_c                   12.2807(3)
_cell_measurement_reflns_used    5211
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.7740
_cell_measurement_theta_min      6.0920
_cell_volume                     1622.46(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'PILATUS3 R 200K Hybrid Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.954
_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    -32.00  13.00   0.50    2.00    --    0.00 -57.00  30.00   90
  2  \w    -22.00   9.00   0.50    2.00    --    0.00 -82.00 -60.00   62
  3  \w    -88.00 -36.00   0.50    2.00    --    0.00 -57.00  30.00  104
  4  \w     12.00  69.00   0.50    8.00    --  100.80 -30.00  30.00  114
  5  \w     47.00 100.00   0.50    8.00    --  100.80 -82.00  30.00  106
  6  \w     73.00 118.00   0.50    8.00    --  100.80 -82.00  60.00   90
  7  \w     62.00  99.00   0.50    8.00    --  100.80 -82.00 150.00   74
  8  \w     55.00 116.00   0.50    8.00    --  100.80 -82.00 -60.00  122
  9  \w     65.00 118.00   0.50    8.00    --  100.80 -82.00-150.00  106
 10  \w     77.00 103.00   0.50    8.00    --  100.80  30.00 -90.00   52
 11  \w    139.00 184.00   0.50    8.00    --  100.80  30.00 -90.00   90
 12  \w     87.00 180.00   0.50    8.00    --  100.80  82.00-180.00  186
 13  \w     19.00 132.00   0.50    8.00    --  100.80 -82.00 120.00  226
 14  \w     11.00  67.00   0.50    8.00    --  100.80 -30.00 120.00  112
 15  \w     21.00  56.00   0.50    8.00    --  100.80 -82.00 150.00   70
 16  \w     14.00  66.00   0.50    8.00    --  100.80 -30.00 150.00  104
 17  \w     16.00  49.00   0.50    8.00    --  100.80 -45.00-150.00   66
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'XtalLAB PRO MM007, PILATUS3 R 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0448350000
_diffrn_orient_matrix_UB_12      -0.1542061000
_diffrn_orient_matrix_UB_13      0.0025057000
_diffrn_orient_matrix_UB_21      -0.0952670000
_diffrn_orient_matrix_UB_22      0.0721876000
_diffrn_orient_matrix_UB_23      -0.0155485000
_diffrn_orient_matrix_UB_31      0.0040667000
_diffrn_orient_matrix_UB_32      -0.0120920000
_diffrn_orient_matrix_UB_33      -0.1246057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9721
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.867
_diffrn_reflns_theta_min         5.758
_diffrn_source                   'rotating anode'
_diffrn_source_type              'MicroMax 007 HF'
_exptl_absorpt_coefficient_mu    16.870
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1464P)^2^+0.0787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2611
_reflns_number_total             3267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00845d2.cif
_cod_data_source_block           cuhmhb
_cod_original_cell_volume        1622.47(8)
_cod_database_code               7232991
_nottingham_internal_coll_name   CUHMHB
_nottingham_internal_coll_number 17671
_nottingham_internal_coll_client HMH/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '8.00, 2.00'
_nottingham_internal_coll_frame_width 0.50
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   08/05/2018
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_process_date 08/05/2018
_nottingham_internal_process_user pcxhh4
_nottingham_internal_solution_date 08/05/2018
_nottingham_internal_solution_user pcxhh4
_nottingham_internal_refinement_date 06/03/2019
_nottingham_internal_refinement_user pcxhh4,pczwl,pczspa
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H25 B Cu F2 I N4'
_chemical_oxdiff_usercomment
'CUHMHB #17671 MM-652 in fomblin on micromount for HMH/DLK'
_reflns_odcompleteness_completeness 98.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 N6-B1 \\sim N2-B1
 with sigma of 0.02
 F7-B1 \\sim F8-B1
 with sigma of 0.02
 C13-C9 \\sim C9-C11
 with sigma of 0.02
 C14-C12 \\sim C12-C10
 with sigma of 0.02
 C14-C10 \\sim C11-C13
 with sigma of 0.02
 N2-C3 \\sim N6-C5
 with sigma of 0.02
 C3-C15 \\sim C5-C22
 with sigma of 0.02
 N6-C20 \\sim N2-C17
 with sigma of 0.02
 C17-C16 \\sim C21-C20
 with sigma of 0.02
 C22-C21 \\sim C16-C15
 with sigma of 0.02
 C18-C15 \\sim C19-C17
 with sigma of 0.02
 C24-C22 \\sim C23-C20
 with sigma of 0.02
 N6-B1 \\sim N2-B1 \\sim C4-C3 \\sim C5-C4
 with sigma of 0.02
 C9-C10 \\sim C9-C14 \\sim C14-C13 \\sim C13-C12 \\sim C12-C11 \\sim C11-C10
 with sigma of 0.02
3. Restrained planarity
 C4, C9, C10, C11, C12, C13, C14
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F7(0.5) F8(0.5) N2(0.5) N6(0.5) C3(0.5) C4(0.5) C5(0.5) C9(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5)
 C14(0.5) H14(0.5) C15(0.5) C16(0.5) C17(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5) C21(0.5) C22(0.5)
 C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 B1(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C26(H26), C28(H28), C30(H30)
7.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              57537
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 2.321
_oxdiff_exptl_absorpt_empirical_full_min 0.663